CA2992310A1 - Dry citrus fibers and uses thereof - Google Patents

Abstract

The invention relates to citrus fibers in dry form having a storage modulus (G') of at least 50 Pa, said G' being measured on an aqueous medium containing an amount of 2 wt% citrus fibers dispersed therein under a low-shear stirring of less than 10000 rpm.

Description

2 PCT/US2016/044226 DRY CITRUS FIBERS AND USES.THEREOF
FIELD OF INVENTION
[00011 The invention relit* tO citrus fibers and citrus fibers hasedcOmpOSition in dry fonn and in particular to such fibers and coinpositions.Which are readily.dispersible. The Invention Thriller Mates to -a method ..for manufacturing said fibersand .compositions and their ..uses.
.BACKGROLIND
-0021 =Citrus--fib.ers are known to have many interesting properties making them suitable for use- in. a variety of products:I-1yr hurnanandanimal consumption,-Citrus fibers have be:en successfully-employed, -mainlyas texturizing additives,in food and-feed.products and beverages,.
but also in personal eare,pharinaceutieal and detergent products. The Use of ants fibers in dry -form (hereinafter 'dr.ye tirtit fibers") itt-the manufacturing Of-the:above products is advantageous d fibei.S.)-Jortgershelf life and reduced costs. of shipping froin a fiber production plant Or storage site to a proeessing-aeility.
[00031. 'Dry citrus fibers and'COMprisitionS containing thereof am for -example known from WO 2006/013697, W0.201.2/0 IWO,: and WO 20.13/I09-74. When carefully dried, these knoWn chins fibers ma retain an optimum free 5urface area available for binding water upon .rehydration and dispersion,. which in turn provides said fibers with thickening capa.billtips, good .541044, and the eapacitylocreateoptirimintextures. Using various techniques such as the one --disclosed in WO 202/01620.1 theproperties-oftbe dry citrus -fibers can be further tailored to = provideoptinaum funetionalities.
-0041 ft is, however (billets It-to pm-paw:dry citrus fibers.
withoutaffectingtheir :dispeoibility in aqueous media. A method of erthancingthe dispersibility of dry. citrus fibers in an-aqueous nteditnn is to functionallgeor dil:theatize,tho fibers, le grafting various chemical Innittics-ntithe surface of thefibos.. US 5,964,910 discloses: dry fihres e.g.
citrus fibers, funetionalited-Withaeidic polysaccharides retained on their surface. These :fiber however( Can only bed ispersed in water with it-high,;Shear Miting device of the -ULTRA
TURRAX typtaiñd Cannot be ihns.00nsidered readily dispersible:
[0005}- Another method known to provide dry., dispersible fibers, inVOIVeSdryina the fibers in the veSernie of additives; US:6,485,767 and US 6,306407 diseloSe dryt OinpoSitiOris containing up. to- 20 wit%:.I.of apOlyhydroxylated CoMpound.and dry fibef7S.
Although Citrus fibers WerenientiOned As being a suitable example, no expetitnental data using such fibersWas reported therein: Aeterding-to the experimental part of these publleations.
Sonteivhat dry fibers (i.e., fibers having a dry substanceet-intent Of about 77:wtWandabinit.23 -Wi%
moisture).
extracted iktin'sugarbeet pulp Were readily.:disperSible inWater. using beily:
vigorous. Stirring (500 rpm)õ FloWever,µ.theõprepertic's of these fibers Can be further optimized, in partieular their moisture content: and/or viscrieWtic Properties, 00061 It was also observed that known-. dry compositions containing citmsfibers and additives may have 'undesirable -characteristics such asstieldnessõ width in tttrn may cause problems during a subsequent processing thereof rso; the theological behavior and viscoelastic stability of such compositions are less than optimum with large variations inQS being observed when changing the nature and/or varying the amounts ofthetompositions'-constituents..
-poi} Aecordingly,-tbere is an untnetneedia-the industry for citrus -fibers in -dry form --used as 51.101 or in -compositions,. which can be readily dispersedinan aqueousinediturt, and.
whichtipOn dispersion provide said medium: with an optimum.
theologietabehavihr, Mort-in part iculer,litte is-Alletd :for illy citrus fibers used as Such or intOinpositiOns, Whielt when dispersed in anaqueonsinedium,provide theaq.ueouS Medium.-With optimum O':-v5lues andlor-an -optimum -visedelastic -SUMMARY OF INVENTION
[00.08I A pritnarkoh*t of this. invention May thus: be to provide dry.
citrus fibers that can, be readily dispersed under low-shear stirring in an aqueousmedium to formadispersion having:optimum theological properties, 100091 lbe--Ibregoingand other:if*jetts.of this invention-are .met. by..
providing citrus--fibers in dry firm. having a. storage modulus ') of at least 50 Paõsaid--6.' beingm.easured onan aqueous medium. containing-an amountot 2 wteriveitru.s :fibersdispersed therein under a. low-shearstirring :a less than IMO rpm,.
BRIEF 1)1 SC oPTIGulois [Nola] Figures I and 2 show NM.R T-7..-distributioneurveS
characteristic:to:Me fibers Of -die invention Upon their diSperSal under speeific-chnditions itt-detailed herein .-..DETAILED DESCRIPTION

[000111 Any feature of .a particular embodiment Of the:pre:tea invention may be utilized in any other embodiment of the invention. The Vvned "eomprisiriu7 is intended to mean "ineltid ing" but not necessarily totisiStinit metimptiodbfn: In other WOrifs., thelisted.stepS
or options need not be eXhauStive,-114-noted that the eXampleS-given in the deScriptioWbeloW
are intended to clarify the inventionand not intended to limit the invention tolhose examples per se. percentages nre:weightAveight percentages.. unless otherwise indicated.
Except in the examples and comparative experiments,-- or where otherwise:wild4y indicated, all .numbersinthis-deseriptlwi indicating amounts.ormaterial-or eonditions of reaetion, physical propertica..of materials and/or use are to he understood as modified by-the word '4thpuf.'..Linim.
specified ()itemise, numerical ranges expressed in the. format limn x to y".are tmdersto.od-1o.
ineltide x. and y.: When. fora specific feature innitiple preferred ranges arciescribed format "Am X to e, it-is:understood that all ranges- combining the different endpoints are also contemplated, Forthe:purposeortheinventiontiinblent(or room) 'temp erattft1S-defined:as a .teraperatureofabenit 20 deareesõ.CelsiuS.
[000121 Ina first aspect, the present. invention provides chits:fibers:in dry font having a Storage modulus:(03tif at least 50. Pa, iµaid.cr being measured-On an aqueous Medium.
-cOntaining anamount of 2 wt% eitrtiS fibers dispersed therein under salow-Shear.stirtinit Of less 'than 10000 rpm, 000131 The storage modulus Ctis..conimonly used in the food industrytpanalyie the theological propertieS of disPersions.anif in particular fiber-based .dispersions. In the: art, by fiber-based -dispersioniaunderstood fibers or COrilposiOckas.wntAining thereof dispersed in an.
aqueous medium. 0' is a measure oradefOrrnation energy -stored in the:
dispersion:during the application ofshear forces and. provides an excellent indication Ofthedispetlion's yiscoelastic -betuiviorõ.Ifere,.-G" is measured on an aqueous medinm containing= amount or 2 wt 4-orcitrus-fibers, 1..e relative to the total weight of the aqueous medium¨his highly desirable to achieve :dispersions having -values as high as possible at concentrations of fibers.
as low as possible when the-fibers are dispersed undertow-shear in:the:aqueous medium, [000141 The :present inventors-noticed that. the citrus fibers of were able to 'meet the above requirements and:hence, thesenOVetfibett may impaitfood., feed., pharma or personal Care forniulationseontaining-thereotWith optintuntrheoltigittil properties. The novel citriniftberS have also an improved dispersibility in that they are readily dispersible in the atittoottS Medium. Moreever, sing* said citrus. fibell may be Used at-lower-COncentratiOnS to ticilieve- increased G' values, fbOd, feed andotherntanufactureis may have increased design

3 -freedom lottheitreSpeetive formulations,-inthat they-Maybe able to add or remove constituents while maintaining optiitinm viseoelastk-Vroperties thereof [000151 As USed herein, means that npon dispersion in an aqueous Medium. e-,fg. Water4 the dry fibers have the capacity tolargelyregain their, initial ftinctionality, wherein by mitral fintetionality is herein understood the functionality Of the.frbers before being.
dehydrated and/or dried. 'Properties defining the initial. functionality may include the fib0.s?
swelling capacity, viscoglasticity, water-binding capacity and stabilization power.
[00016] 1 he term 'readily dispersible" het.* means that it is not necessarrto use õhigh-shear .means, e,g, high-shear mixers-or homogenizers, to-disperse-the fibers in an aqueous -medium such aswaterinordertoohmina .usefut viscosity; but rather that the dispel-Sinn of the fibers can be-aceonmhshcd.wi.tblo*,shear-stirrina equipment, such as for example,: magnetic.
stirrers or mechanical stirrers, e.g. 'an 1.K.At 'Eutostar mechanical stirrer equipped :with anil 042.

4-bladed propeller stirrer or a $ilverson L4RT overhead batch mixer equipped with An Eingisor Screen (e.g. with round holes of about 1.1mm diameter).
. [00017] T.hetetin "agneousinediune as used: herein Meat* a liquidniedium whit*
tontains.watet,Suitable non-limiting example thereof includintpUre Water. a .WatersOkitiort and a water suspension.
[000181 The G' the. Citrus fibers of the invention IS at least 5.0 Pa.
Preferably.-said G' is.
at least .75 =Pa, More preferablY at least 100 Pa, even mote preferably at least 12$ Pa, yet even morepreferahly at least .150.-iPti, Most preferablY :170 Pa.
[00019] Theinventors surprisingly observed that the chi* .fibersof the invention . manifest-the. high G': values upon being dispersed in an aqueous. medium undertow . stirring with less than 10000 rpm. This is even more surprising .since said high G' -values were -achieved at the low fiber concentrations, e.g; O12. The aqueous medium preferably cpatains-water in an arnountof at least 75. wt%,_ more preferably:at least 85 wt%,. rngst .preferablyat 'least-45 relativetothe total amount- of the medium. Preferably, the stirring used to achieve the dispersion of the fibers of the in vention in the. aqueous medium is Al: most:
8000 rpm. more preferably-attnost :5000 rpm, most-pretemblyat most 3000-rpm.-[000201 The citrus fibers of invention- are in dry form which is herein understood as containing an 'aritritint of liquid,. e.g. 'water and/Or Organic solvent,.:ofleSS thatt 20-wftrelative to the total Weight of the fibers. Preferablysaid fibers contain an ambunt of water (i.e. moisture -eenteritytifat most .wt%otuirepre.tferably at most 1:0 Wt%, OrItioSt preferably at most:8 Wt%:.
.Stieb dry fibers May be mote econbinital to transport and store Wtiic being readily diSperSibk. in the aqueous medium [000211 The fibers Of the invention are citrus fibers:. ThefertitheraS used herein, refers to ati elongated object comprising microfibrils of Celluloseõ-the -fiber having a. lenuth (ma lor akiS) arid a Width-Oninor Axisykold having length .to width ratio of at least 5,- more preferably at. least 10; or most preThrablyatleast. 15; as observed and measured by A high-resolution Seinnittit 'electron irrieroseepe (WNI".); The length Of the -Citrus fiberS iSpreferably at least 04.10, ITIQre preferably at least prit The width of the chruS fibers is preferably at Most 100 run, more preferably at most 50 Mu, most preferably at most 15 nrn, [00022] Citrus fibers are fibers contained by and obtained from the fruits Of the Citrus:
family ,-The citrus Wilily is a large and diyerse family of flowering plants, The eitrus;fruit is considered to he a specialized type ofberry,.characterizedby aleatherypeetand alleshy interior containing muhiple ettons filled with juice filled sacs, 'Common varieties-Utile:Atm .fruit -.Maude oranges,.sweet-oranges, clementines,. ;kumquats; tangerines, tangelos, satsuma*, mandarins, grapefruits,. citron*, pomelesõ.lemensõreugh lemons; limes and leech limes: The citrus fruit maybe early-season, rnid,season or late-season citrus fruit, Citrus Alas also contain pectin', common 'ID fruits but fotindin particularly high concentrations in the.eitrtis &nits. Pectin is/agel-fortning-polySateharide With a terrip Strilettire.-.11 is essen tia ly.made of partly knethokylatedgalaCturonic acid; thamnosewith:Side chains Containing arabitioSe and galactose, *filth are linked through a glyeosidie linkage:- The peetin Content of the citrtialluit may vary based dn soaStm., ?Where ripe fruit May Contain less:peetinthatt oeipt fruit [00.023 Citrus. fiber is to be distinguished fromeitrus Pulp, which:are whole juice:sacs and are sometiMesleferred-to as citrus vesicles,, coarse pulp, floaters, citrus. cells, nearing pulp, 'juice sacs or pulp, 'Citrus fiber is also to l)distinguiShed from citnisrag, which:is:a:material -containing segmentmembraneandeore of the citrus :fruit The citrus fibers are-typically:obtained-from a gmrce,:of citrus fibers; e,g, citrus = peel, citruspulp, citrus rag or combinationslhereet-Moreoverõ the citrus fibers may contain the components Oft primary cell. walls of VOUS fruitstich as cellulOse, pectin and hemiceihdoses and may t150 Contain: proteins, [000251 Preferably; theeitrus-,fibers of the invention did not undergo any substantial chemical ruodification,le said fibers were notsubjecteditothemical modification processes such as esterificatien, deriVatiSation or tniyMatit. modification and cOrribinatiOnS thereof:
[00026] Preferably, the aims fibers inaecordance with theinvention.haVe a crystallinity.
.of at least 1.0%, mero.:prefeMbly.dt least 20%, most preferahlyat least -30%aS measured. ona dried OeSS dian20 *t% Water content relative tothe .t.õ.binentof fibet.$) sample by -X-ray di ffractiOn method.(Siegel method); Preferably, the crystallinity:Of Said.
fibers is 'between 10%
and 00%,.

[0002.7] The inventors- surprisingly found that suitabiy prepared citrus.
fibers-in. dry fOrm can be readifydispettedinatt aqueous medium by applying relatively low levels Of -shear compared 1:0 eormilitiotia1 dry citrus fibers. Without. WiShing. to be hound by thebry0t is believed that the -ekeellent -diSpersioir properties ofthe citruk fibres are-Mated to the structure that is :imparted on them in the drytbrinAt WaSltirther trirpriSingly found by the.presentinVentorSthat this, structure can suitably. be characterized by a standardized shear storage modulus. ((14') that is :.determined. for a standardized dispersiOnotsuch citrus fibers.
[0002.8] Consequently; according to a second meet; the .present invention .provides, citrus, fibers, in dry form having a G* of at least 50 Pa, wherein -GP is measured by:
a. mviding The fihers--inAparticulateform wherein the particles can pass a .500 gm:
sievehymillingthecitrus fiber .m*00 using a Waring 80:i(i.E0 'laboratory.
'blender equipped witban SS-I to PtilverizerStainiess :Steel Container using its low speed setting (.18000.rpm) for 4.:pfus or minus It seconds;.sieving the milled material using.-anõ AS200 digitalsbaker from RetSekOmtilI Germany withu sieve set of f0rnm-5001tin,2:50p.in and 50 IIM sieves,. whilst shaking for I Minute at an.
-amplitude-Setting:of 60;- remilling and regevingthe.partit les larger than .500 pm until -they-passed the -500.-AM sieve and cOmbiningthe-Sieved fractions;
h. dispersing an amount of the 'fibers iii particulate-Rum so-as-to-Obtain 300 grams of an *wogs dispersion comprising...2 wt!%.k of drY-CittuS fiber by *Oleg- 'of the 'dispersion, "4ellerein the dispersion is buffered at pH7.0; and wherebY the fibers are dispersed using a Silverson overhead Mixer equipped with araZmulsor screen baying round holes, ofl mm diameter at 3000 rpm for 120i scronds; and e, determining G* of theresultant dispersion using a parallel plate rheometer, -[0.0029.] Step a. of the above protocol for-thedetertnination-of serves to facilitate:
ctiwient-diSpersion during step 4..Tbecitrgs.fiber in dry -form may comeata variety of partiele.
sizes. Therefore, step 'a. includes milling of the citrus fiber so as. to obtain the fibersin-lhe specified partieutatelium. Suitable milling is' provided by dry milling.usittgalahoratory-seale Waringiblender. The buffered: dispersion. of stup b. may he:prepared-using-any -suitable buffer.
systeM. Prefereibly, a phosphate-based buffer is Used. In-Step c, the Silvertorroverhead mixer preferably:IS-art 'ART overhead Mixer. G ismeasttred using anrauitable-parallel plate-Theo:MeV:1k, km example. an. ARG2 theometer TAInstrintients. G:* is preferably Miki.stiNdat.a.
sham level of 0. I% .A preferred. of establishing the G* is by 'folloWingthe protocol in the way deseribeir below. The above protocol and the EXatrtples.proifide methods Of measuring the G*.nowever, the-G4may'also be determined hY a difitTent prOtocot,..451.oiwisINitprptostal 6:

Would lead to the samephysical result; i.e. -it would yield the same (3** for a particulardrytintia .
fiber 'preparation As the aboveprotecOl.:
[00930] The citrus fibers in dry form according to the second aspect Of the inVention preferably have a Cr Of at least. 100. Pa, more preferably- at least 150:-Pa, even more preferably at = least 200 Pkatill more preferably at least 250- P4, and yet more preferably -at leaSt 300 Pa and even tnore Preferably at leaSii3$0.Pa: The eitruS fi ben in dry form Preferably ita*.ea G.*: of itp to 10000 Pa, and more preferably Our) to 1000 Pa. Thus it is particularly prefertedthatthe citrus fibers in dry form have-a- 0* of between 50 Pa and 10000 Pa, more preferably betweetf.3:0() and WOO Pa.
[0093.11 Ina third -aspect, the present invention provides a composition of matter in dry :NIA comprising citrus fibers and an additive:distributed between said fibers, said composition havinga.storagemodalus (07).of at. least 1:90:Pa, said Wheingneasured on an aqueous medium obtained by dispersing therein an amount of said composition ander a low shearstitringõ
ofiess than 10000 rpm to obtainaeitrus fibers! -concentration. of 2 witi*:
relative to the total.
weight of the aqueous:medium. Preferably. CI' is at least 130 Pa, More preferably .at least 170 Pa, even more preferablyat least 190 Pa,- St even more.prefrablynt least-250- Pa, yet even Mere preferably at le451.3-00 PE4. Most- preferably,a least 350 Pa when said composition is dispersed Under a loW:shear stirring of -legs than -5000 rpm.i more. preferably less than3000 rpini- Preferably, is at least "37$ 'Po, Mate preferiblY atiettSt.425.Pa, eVOtt inbre preferably at least 475 Pa, Y'et even more Preferably at le* 559 Pa, yet even More-x.00ra* at: least .600 P1.1, 010St .prefer.a.10 a(least 650 Pa when said composition is dispersed under a low -Shear stirring of between 6000 and 19000..rpmõ more .preferably between 7500 and 8500. rpm.
[0.0912) The compe.sition of the invention hereinafter the inventivecompo.sition,:ig:in dry form, which is. herein understood that the composition emitting .an Am-twin Of water andior monk solvent,nfless than '20 wt% relative to the:total weight of said .composition.
'Preferably-the composition contains an amount of of at most 12. more preferably at most -wt%, or most-preferably gt1T10St 8 wt%. -Such a:dry composition may benfort:
economical to transport and stare.
[000331 Theinvetnive composition eompris.es an additive distributed between. the ohms;
fibers: By the term ."addittiv distilbtded behteen the citrug libers"ls herein understood that said additive is distributed inside a volume defined bythebtality Of fibers and preferably also bet*ecitthe -microfibtils frirmintthe fibers: Preferably, the tints fibers used in the inventiVe eottxposition are the chits fiberS-iofthe inventiOn.
[090341 Preferably, the inventive composition 0,61144 the additiveinan amonnt..of:at.
least 5 wtoeil. relative to the weight Of the .anhydr.ous citrus fibers contained by said composition.

more .pirefetablyof atleast: 10 WeS,, ath more preferably Of at least 20 wt%,..Or most preferably Of at least 30 wt%. The weight f the .arilirritons frbers.in-the composition is the *tight Of the.
fibers obtained by drying .10 grams of therzoinpositionwithout the 'additive at 105 under normal atmosphere anti! constant weight iS -obtained; The same determinatiOn can be carried out.
in the presence of the additive; :however, in thi ise the amount of additive in the sample has to be subtracted therefrom. the upper limitl.1hrthe additive amountintheinvernivecoMposition can. be kept within large variances! since it was Observettbattbecitrus.fihers cootaine.d by said composition may have the :ability to optimally ,include saidadditive, A
preferred upperlimit for the additive amount Isat most 1.000 wt% relative, to the weight of* fibers -in:said-compositien,.
more preferahly-at most 750 wl%, or mostpreferably at most 500 wt%..
-100035] 'Preferably, the:inventive composition has an .additive:fiber (AT) ratio. of between 0.01:1.0 -and 10.0:10-by weightortorepreferablybetween and.
9.01.0 by-weight, DIM
preferably between 0õ41,0 and $.0:1.0 by weight. Inalirsternhodlinent, the=Az12. ratio IS-between 0.011.0 and-3,8: 1.0,.more preferably between,0.05:1õ0-and 3.4!1.0i.
Most preferably between 0.10:1.0--and-3 Ina second.embodiment,.the A:17 ratio is between 4.0:1.0 and 10:O.: IA more preferablybetWeen 4.5:1.0 and 9.0:L0, most preferably between

5.0:1-.0 and.
iiiveritorS observed that the inventiVe composition his stable theological properties = in that when Varying* AT ratio Of the composition, the G' gat* With a Standard deviation (MEV) of at Most .50%-of a Maximum (MAX). wherein MAX is the maxim Measured value of*
[0000] For compositions comprising additives and fibers, 0' may depend on the amount and nature of the fibers but aisp.cm the A4F ratio, In Other wortis,.a.composition with a specific:
3,7 ratio ha $ a: specific G' andby changing said ratio; G' thanes -Also,. The amount with which chanes.wjtiythe.A:P ratio, e.g. as expressed. humps of the: standard deviation (STDEV), may give, an ind1catienof.the dispersibility and the thee-logical viscoelastic) stability of the -composition, [000.371 Theinvetitors- observed that While changing the A :17ratio of the inventive composition, mayexperiericea Maximum (MAX).; And thatthedeviation expressed as.
STDEV Of =O' from MAX for -VatiOnS A:F ratios May also givtahindieation on the-dispersibility :and:the rheologidril Stability of the composition. They Observed 'thatan increased deviation of STDEV front MAX May deleted-Way inflamed-the processability Ofthe.composition as processing steps with StarklY 'different :setsbfparameters- may be required for eachA:Fratioin order to achieve an optimal pmeessing thereof, The inventors also Observed:
that eirioto characteristics of composition such as shelf stability and sensory perception, inglading ...texture and mouth-1W May alsebe negatively influented by tutittereaSed deviatiOn OISTDEV
from MAX.
[000381 The inventors observed that in the known ctinipoSition.s, additives were tidt:
efficiently tribted With said fibers,. which May re.sultinalesseptirnaldistribtition fthe additive 'between the fibers. This may refleeted by the eompositione teSS Optimal theolOgiCal :behaviour, .e.g. large variations oftiteeompositionS' With the AT ratio and in particular large :deviations of filDEV from. MAX, [0009] for the composition of the inventionthe-STPEV-charaeteristic to the G' variations is at most 50% of the MAX. Preferably, the STOP/ :is at most 40% of said MAX, more preferahly itt:most 30% ol said MAX,-eyen more preferably at illeSt 20%
of said MAX, most preferably at most. 10%0 said MAX.. Theinventiyeeemposition:mayalso he considered readily dispersible. Moreover, the inventors Observed- thatiWiten.the A ratio is varied, the obtained values are closely groepedaround the MAX; hence- the. inventive -composition may have aViscoolastie behavior-which is less dependent on the (.1,0ncentrationand/ornature of added constitut,'nts.:than known Citrus fiber-based compositions and May thus OfferinereaSed design freedom .forprodutts- whose: theological Or otherproperties are modified Withthe help of these citrus fibers.
[000401 The additive used in the inventive COMP6Sitidn, is preferably chosen from carbohydrates and pelyols. CerbOhydmfeS inchtde also dethativeS-thereof .Preferred carbohydrates are linear oreyelicinonosaccharidesõOligosaccharideSõpolysacc.harides and fatty derivatives thereof. .Examples of fatty derivatives. may include SucroeSters or fatty.acitt sucroesters, -carholi.ydrate alcohols and mixtores--thereof Non-lintiting examples. of õrnonosaccharidesinelude fructose, mannose, galactose, glucose, *lose, guloseõallose, altrose, idose,.arehinose, xylose, lyxose and -ribose. Non-iimitingexamples-ofoligosaccharidesinelude sucrose; maltose and lactose. .exam.plcsof polysaccharides include nonionic polysaccharides.; e.g. galactemannans, suthas guar man, carob gum, starch and its non ionic derivatives, and nonionic; cellulose.derivativm- but also an ionic polysaccharides such as xanthan gum. At/coin-tidy:0ms,, carrageertans and alginates. Preferred examples of polyols includewithout limitation klyeetol, penitierythritolõ- propylene:glycol,. ethylene &yea and/or polyvinyl alcohols.
The additiveSennmerated above can be used alone Or in naktures.ot blends oftwOOr Mere additives.
[00041] tn apreferred embodiment,. the additive is al:hydrophilic additive, suitable examples incltidine dextrinS; water-Soluble Sugais such as glucose, Trude*, .auctrise, lactose, = isinnerizcd Sugar, xyloSe, trehaloseõ:a.mplingSuger,..paratitioie,..sorbesei..reduCed Starch-saccharified ginten,:intaltoSe, hietulose, fractooligoSacclitirides,:gilaetooligosaceharik-.

hydrophilic starches and 'sugar a:Who's such as xy:litok nialtit01, mannitol and sorbitell WAS
combinations alma [000421 In another preferred einhodiininit, the additiVeis. a starch.
Thestatch used. inthiS
itiVention may be any .Stareh.deriVed from-any natiVeSouree, -A bath-est:tech as used herein, is.
one as it is found in nature,. Also..stantbleart. taithes deriviAl frem aplant Obtained by any known breeding:techniqueS..TypicalsoirreeS for the Starches are CereakS,::mbersanifroots, .legumes and fruits. The native source can: be any variety,. including without limitation, corn, potato, sweet potato, barley, wheat, rice, sago, amaranth, tapioca. (cassava), arrowroot, canna, pea, banana, oat, rye, tritiqile, and. sorghum,.aa wellaslow amylose ( waxy)=
and high amylose varieties. thereof, Low arayitise or way 'varieties is intended lo.mean a starch containing atinost 0% arnyloseby weight,..prekrablyat most 5%, more preferably attnost2%:andmost .preferabiyat most I Watnylose by weight-of the starch. High atnylose varieties is intended to mean a starch-which contains at least 30% antyloseõpreferabiratleast:50%-amyloseonore preferably at least 70%antylose, even:more preferably at least 80%amytose, and tritist preferably at least 90% amyiose;all by weight .ofthestareh. The -Starch may bephysitay -'treated. by any method known Iii the art.to.mechatileally Sher the-Shirckstnittas by: Shearing:or by Changing the granular or crystalline nature of the starch, and as. used .herein is intended to =
include conversion and pregelatinization. Methods of physiCal treatment: knoWn in the:art include homogenization, high Shear blending, high shun coOkingtnch as jet cooking or in a homogenizer, drum drying, spray-drYingõspray hdsonation roll-milling milling and extrusion, andtherintil treatments Of low .(e,g, at most. 2 wt.%) and high (above 2 wt%)moiSture containing starch. The starch may be also, chemically modified by treatment with any reagent or combination of magentsimownintheart, Chemical modifications are intended to.
include crossiinking, acetylation, organic estercation,organieetherification, hydroxyalkylation (including hydroxypropylathin and hydroxyethylation), phosphorylation, inorganic esterificatione. ionic (cationic, anionic,nortionle, andzwitterionic) modification, succination andsubstituted saccinationof pelysatcharidesõ: Also included are:oxidation and.
bleachingõS itch nitidifications- are known in :theart, for example in Modified starches: Properties.
and Uses. Edõ.*.ttrzburg, CRC Press, inc., Florida (1.9136), [000431 In-another -preferred enihodirnent, the additive is A blend containing,:a first :-additive and a second additive, The -fitiit additive being a starch ad the second additive-beinga carbohydrate, a derivatives thereof or -a .polyol, -Wherein the. seeond additive is different than the first additive Preferably, the starch IS *Nista:1'oeifl the:grotip of starches' Containing:a...tiative Starch, a thermally treated stareh,a chemically modified: starch and combinations thereof.

Preferably, the second additive is choSentkOm the group con-sitting:of glutOse, sucrose, -glycerol and sorbitnl..
[0004I] Most.preferred.--additiVes forase in the inveritiVe composition arelliteoSe, sucrose; glyeerOlarid-sorbitot 1000451 The inventorssurpriingl tbund that a Suitably prepared composition of Matter In dry formõ-cornntiSing citrus fibers and an additive distributed betweensaid .fiberS:Can.be ..readily dispersed inart aqueous medium by applying relatively low levels of shearcemparedto :conventional dry citrus-fibers. It was: further surprisingly found by .the present in ventorsthattbis . structure can suitably be eharacterisedby a statulartlizediriodulus(G*) that is determined for a standardized dispersion of the composition of:matter,. Consequentlyõ.according to a fourth aspect, the present inyeation provides a-composition ofniatter irtdry form comprising citrus -fibers and-an -additive distributed. between said fibers, said composition havinga G-* of at least 150 Pµwherein.G4 is measured.by a; providing.the:compositiOn-in.a particulate form wherein the. particles can pass a .500 Am.-sieve by Milling the citrus Material Wing a Waring 8010EG
laboratory -blender equipped with an-SS110 PulVerizer.StainleSS- Steel-Container using its low speed setting .(18000 rpm) for. 4 .plus or minus SeConds;
sieving the Milled material using ari-AS200.digitg Shakeffrom -Retselt.GmbH Germany with a sieve set of 1-0Mm, 5000M-, 250AM and.50Ain SieVeS, v=VbilSt:-Sbaking for 1 minute at an amplitude setting of 60 reinilling and resieving-the particles larger -than .500 Ant until they passed the $00 Am sieve and combining thesieved fractions;
dispersing in amount .of the composition in particulate:1*m so as to obtain grams of an aqueous dispersioneomprising 2 wt% of dry- citrus fiber by. weight of the dispersion, wherein the dispersion-is-buffered at pH. 7.0, and. whereby the fibers are dispersed using a Silvers.on overbeadMixer equipped with an Emulsor screen.havingrourni holes off nun diameter at-3000 rpinfor'120 seconds; and:
c. determining .G*- of the resultant dispersion using ..a parallel plate rheom der.
[00001 Step a. eftheaboveprotociA for thedetermination.of Gs serves to facilitate efficient -dispersion during step b Thetornpositinn of matter in dryform nitwoonte at a variety .dfitrticlifSies Therefore, step a: incltidesniffling of the -coinpoSititm so as to Obtain, the fibers in the. Speeitiedpartictilate forth. Suitable Milling is provided by dry-Milling using a laboratory-Seale 'Waring blender. The buffemd dispersion Of -step h. may -be prepared using any $iiii4blt :buffer syStent. -Preferably, a :phosphate-based-OW* is -used.. In step c, theSilYersOnoverhead -1õ1 miXer:preferably is ata4RT-OvetheadmiXet measured using. any suitable parallel-piate rheometet;for exalt* an ARG2 theometer ofTAInstrantentt. G* is preferably-measured-at:a strain levet of 0:114,-A preferred Way-ofestabliShingithee't iaby-felloWitiathe protocol in the way described below. The above protocol and the Exattiples proVide.inethOdS
ofineaSizing the O however, the G-* May also be: determined .by a different protOCOL-aslOrtgaithat.protoc61 'would leadtoThe same phySleal result, i.e.- it would Yield-the same Cr* for n Partieitlardry citñts = fiberpreparation as the above protocol.
[00047] The-composition ormatterin.dry ft according to the fourth aspect of-the invention preferably .has ad* prat:least 200 PtL more preferably atleast:250 Pa, even more prefernblyat least 300 Pa:and still-more-preferably at least 1.50 Pa.
Thecompositioneftnatterin dry.fitm preferably has-a:0*--of Up to 10000 pa, and more preferably of up to 1000 Pa Thus it is.
.particolatly -preferred.thatThe composition of matter in dry form has:a G.:!t of Pa and 1600.0P0 more: preferably between 3001 Pa. and 1000 Pa.
[000481 The :preferences and examples -regarding theeltrus.fiber, The type and amount of additive in the composition Of matter ateerding.tothiS!fottrthaSpettOf the invention arc as presented hettiriabove for the corapOSition of Matter in dry-forth Comprising citrus -fibers and an :-additive distributed between Said fibers according to thepresent-hwentioit-ft is:particularly preferred that the additiVe is sucrose and that the ratio A:17 Of additive:46 eititS fiber iS 0.10 to 1.0 and 3:0tO 1-.0 by Weight:
[000491 in a .fillh aspect, the present inVentionprovides cellulose fibers in dry fonn having:atianSverse relaxation' factorrRe") is Measured by nuclear thagnetic resonance e'14101r). of at least 0,05. -Tbepreferred-cellutose fibers arc citrus fibers, ere fera.bly, tbeR:2*: of said dry c.ellnlose fibers-is at least 0.70, -morepreferably at.least11,-80, even .more preferably at least 0.90,y:et even more preferably atleast 1.10, midmost preferably:at least 1.20. Preferably, the moistnre. content- of the -dry-cellulosc fibers-is tamest 20 wt% relative to the total mass-of -fibers, more preferably at most 12 wt%, even More preferably at-most 10.
w0.4, most preferably at most 8 wt%. To inventors': knowledge,2cellidose. fibers and in particular citrus fibers: dried to a -.moisture content below theahovemetuionedarnouuts and having the Re in accordance with the .'invention were new trunitacturedbithertoõ
[000501 The -inventors -stirprisinglyobServedthat R2* May be Used to characterize and deseribedry.cellulow fibers andirt .partieulat dry eitrtia fibers. Without being bound to any theory, it IS-belleved that Re trtayproVideanindkatiouttf the magnitude of the aVailable Surface area of the fibers A higher .R2,' thttS-signifieS A largeravailable Sairface area of fiber, whieh in turn may indiCate anincreaSed textitrizing capacity-of-the libers i e the ability of the fibers to fotht and/or stabilize textures It was .9bserved that .ke value*
Such those chaPadefiqic .for the-fibers Of the inventiOtt, were never achieved hithertO, as the publicly -reported values andthe ineaSured valties of anycommereial products existent so far are=well :belt)* 0,-65-.1t i. thus believed that the known dry- cellulose fibers and in =particular the :kiiown=
citrus fibers haves less than optimum. tekturiiing Capacity.
[000511 The in ventorS surprisingly found that Suitably prepared citrus - fibers m dryform can be readily dispersed in an .aqttuous medium by applying relativelY=lOw levels. of Shear compared to conventional dry. 0044 fibers, Likciyi.s.eõ it was surprisingly found that redispersion.
of suitably prepared composition ofmatter in thy km) comprising citrus .fibers and an additive::
distributed between stud fibers can :be dispersed even more readily,. Without wishing to be bound.
by theory, it is. believedthat the excellent dispersion properties of citrus fibersorsaid.
composition inchy form are related to the .strueutre...thatis imparted on them in the dry form, It was. further surprisingly found by the present inventors that this strueturetan suitably be characteri.4e4 by a Fiber Availability.Paraineto (PAP). This iinditqappliesto 'both-the citrus fibers in .dry form and to the composition of mattet in dry form., TheõFAPis measured using a .technique baSeitiOn NNW.. Therefore, .aceordingto.a Sixth aspect, - the itiVentiOn provides Citrus fibersin dry forth having a FAP of at leta-0.3.5 ll.Shnitarly,acebrditig to a seventh aspeet,:the invention provides a composition Of matter in dry form. comprising =citrus fibers and an additive 'distributed between said fibers.havingafAP:of at least 1110-11g., [000521 The 'PAP
is determined in oSSentially the Sturm way. for both=Ihe citrus fibers according to the sixth aspect and the. composition of matter in diy..fortn according to the seventh aspect of theinv.ention. Therefore, the territ.ffeitruS fiber material" is herein underStoodlorefer to either the citrus fibers.. in dry form according to the sixth aspect of the compoitiQn. or matter in dry fOrtn comprising citrus fibers and an additimdistributed.between aid fibers according to the seventh- aspectof the invention, as the case may be FAPprov ides A
measure tbr the internal configuration of the. fiber material and the extentto which the fibers are available for rediSpersion at row shearlevelitts a result-of that :coufiguration. The FM' isbased on the.
-1410.methodperfOrined on -astandardized sample comprising thechrus fiber :material dispersedforin, ThefAP-of the citrus fiber material .1S-estab1ished by thelalowing-protoeol.
The:protocol-to establish-FARincludes three parts isamplepreparation,fNMR.
measurement to colteet-Carr-Purcell-MelbOom-0111-(CPMG)..re1axation decay data, and. data analysis to calculate .the TAP Value, Thus, the protocol includes the sample preparation steps of:
a: :providing the eitrint. fiber .material in a particulate form-wherein the particles canpasa.
500 On sieve, b) millingthe Ciititts fibre Material tigdg:twariii$-s010E(1 laboratory 'blender equipped .NOth.-- an S$11 q.Ptilyerizer Stainless Steel.Contalner using its low 'speed:
setting (18000 rpm) for 04 of minus I seconds sieving theMilledniaterial using an AS200- digital shaker itothgetseltUnibil Gerniany with. a-Sievefsetvil Omm, 500pm, 250gritand 50 gm sieves. *hilst-shaking. for 1 minute at an amplitude setting.
of.60;
rethillingand resieving the particles. larger than 500 Urn until they passed the -500 gm sieve and Combining the sieved fractions;
b. = using the eitnakifiber material to prepare 300 grams ofa concentration-:standardized .sample in the forth of -a dispersion at room temperature, wherein the .concentration-standardized sample com.prises the ,fihers contained in the eitrus fiber material at a concentrationof:0.5awt-%witlyrespect to* weight of the standardized -santple;..hy -:first combining :the citrus fiber material *ittkviater to pin-a-tot:Al weight of 250 sramsõ
optionally adding a preservative, adjusting:The concentratitmotthesample to a pH of 3.6 0,1 using:aqueous hydrochloric acid an4 adjusting the volume of the resulting:mixture -toatotat 300_ grams.by.adding. water;:
C. evenly diStributing.the- fibers inside the eon cc n tration-standardizedsample volume by Agitatirigthe Sample using a Silverson overhead mixer equipped-withan EmulsorsCn.hm haYingtotind holes.al .mm diainetetat 1500 rpm for 120 seconds;
-adjtiSting-thepH.of the. concentration-standardized-Sant* to 3.3 0.1;
e. Ittulderring .attalignahlthe eoneentration- and p11-standardized Sample ton .flat-bottom .NMR tube of 10 mm diameter, ensuring a:fill-height such that upon placement-Of the Satinile ih the NNIR speetrotnetefof Step h, thefill height is within the region Where the -RIF field Of the Oil of the NNIK spectrometer is hotitogeneons, [0005;3] Stepa of .the...0ovskpro.towl for the determination of the .fAy serves to facilitate.
-efficient diapers* during step b. The citrwtiber tria1eriiil may come at ayariety of suitable particle sizes. Theret*e,step a. includes thilling:of the citrus:fiber:material so:as:to obtain the material .in the: specified particulate form_ Suitable mifling is provided by dry milling using a laboratory,scale Waring blender. Thesample- isreferably -kept or made -free from larger .particulate material, including for Instance fragments of whole or multiple cells and othernou7:
irOttiOstotind engteriat The distributing_ step.. c is intended to provide:an eVettAistributiOti of the fibers over the sample volume, whilst having a controlledieffeaort-theavailability of the fibers for dispersion. in step d, the:pi-Lis suitably standardized with thehictethydrochloric acid. The optimal fill height instep einay depend on the tyljt of NNW
Spectrottiettrused, as knoWnby the Skilled person. It will typically be about 1 em. In the further steps of the protocol, the.
-eotteentratioti- and pH,standardized sample will be.referredtn ea the Standardized -saint*, [000541 The data analysis requires. comparison Of- A.1'2 distribution curve (see beloW)Of the standardized sample with .a matrix retYrerteesaittple Which should preferably beeSSentially free from 'cellulose fibers,-Therefore, the .protocol afar) itithideS the Atop' Of:
f: preparing a matrik reference Sample by tentrifirging an aliitiot of the Standardized 'Sam* in. a 2 ml = EppendOrf Cup ita relitiveeentriftigationfOrce. of 15000 fbr 1ff Mintires.
and transferring theSuPernatant to a flat-bottont.lsiMR Mho of 10 mm diameter, ensuring fifi height such Mat.tipon placement of the sample in the NMK spectrometer of -steRk the fill height is within the region where the Id: -field of the Oil Of thy NMR
.spectrometer is homogeneous.
Sphsequently, to-collect:and analyze the data, tbe protocol. includes the steps of::
g, quilihrating :theigly1R. tubes at a temperature of 201-#C;
K recording relaxation deicarditta for:the. standardized:sample:400. *Cowan Wk.
spectrometer:operating:at:a proton resonance frequencyof 20 using g relaxation pulse sequence,.with.a 180' pulse spacing of 200 microseconds, and an.,..cyclo delay time Of3.0:ActOnds;
1. TeCordingrelakation '&0y-data-for the matrix reference sample under the same conditions AS in Step 11;:.
j. perforining.itiverat LapbeetratisforMation to the Obtained deCay.darafor both the standardized Sample and the Matrix reference sample reqtriiing Tz-to be in the range of 0.01 to-l0 -seconds;
k. identifying in the 172, distribution curve of the Standardized sample the peak corresponding to the water protons of which theft: is averaged by exchange between the Milk water phase aridthe surface of the defibrillated primary cell wall material.and identifying .in theTt distribution- eirrsteof the :midrix.referenee-sample the peak -corresponding to the hulk water phase;
1. calculating T (sample), Which isdefined as the weightedaverageTrvalue for the.
:identified peak in the.].T: diStrihation clove athe standardized saniple:andsitnilarly-ealenlittingT:.k (matrix) whiehis defined as the weighted average -7172 value for the identified peak in the:Tz distribution eurve..of the' matrixretereneesarnpie;.

in. ad:nil:ming the values of R:2(Sarnple) and 11,2(matrix), *h&c =Rple)":z 1 I T2(sampte); and RArnarrix) 1 / T,2(nuitrix);
calculating theTAP.Of the fiber mass as PAP-- lt(sample) R2(ntatriX), [000551 The CPMG Tz relaxation puke sequence is w.c11-knOwn in:the field Of NMR
spectroscopy (See f z fdfJsIwumfreeprecesskm in Mide42rmagifetic.i'e's'ondh&
:expithrients, Carr, ILY-.õ:.Pareell, ISsue..-3-,.1954., Pages: 630-.638 tAlodifkd kpir&echo method,* miuthimiirig iniciew' -Ada:WM*
Revrew cy-Scfrolt* 10.0140gots, VOlatim-29õ:1SSUe:8,-.1958,- PageS:688.-691),.:Sultable time domain =1441ViR spectrometers to PerfOrtn this-tYpe Of .spectroscopyare.-wellAnown Sintilarly.; the usual measures to ensure the recording, of reliable data are weil4crtown in the field of time domain NM.R spectrescopy-forample,-the.electromagnetie -field should be sufficiently homogeneous at the locus where the sample :volumes are placed. The. field homogeneity can for e4ampleshe checked by verifying whethera reference.sample-of pure-water,.
yields a T27.(T4wo.-star) for waterprotons :of More than -2 ntilliseconds, Theinverse Laplace transformation of step may:suitably be carried out using anon-negative least-.squareconstraints algorithm Isgnormeg (Lawson,-C.L'and.R.l. Hanson, Se.ilying.Leeut Sqliares.1401)104.,SProVicOliill, 1974, Chapter p. 1:61), with the regularization parameter lambda-set:10Ø2,.
Softwarepackages-suitable for implementing the algOrithm and carrying .out-theltatisformare we-kr/6%4M, .Matiab being an example-of-Stith sofiNVare.
[00056] In step k the peak That is selected in theta distribution ettrve-Orthestandardized-sample, typicallyis the -dontinant peak, if thesyStem. is sufficiently luirnogeneotts. In general, the peak that:Should beseleetedialhe Tzdiatributten enNe. is'that CorrespondingtomaterprotonS of which -the f is averaged by diffusion and Chemical exchange between hulk and Sur4.6e.sites:.of the dispersed citrus:fiber materiaLThispeak is:particularly- Well-defined-ifthc.cittias fibre .material is evenly distributed-over-the standardized sample in most typicalcases, -them Will be only one-suelt peak, as can be spenin.the -examples :in .the Examples soclion below [00057] lbe weighted average Tin step 1 is for example suitably calculated bythe summation.
I Cr2) E. 1(T2) [000581 liete,..1(Ti) is the intonsityatvalue Tzand -both summations .areovetthe width-of the peak.
[000591 A .preferred Way:Of establishing the FAP for the-nitro-4 fiber material is 'following th-eprotetol in theway described in.theExaMples section below. The above protocol and the Examples provide method of ineaStitina thefAR- However, the'FA.P May also be determined bYaditTerent prot66.11, a Ring as that protocol *mild lead to the Same physical *nit' l.e, it4O.old yield the. same PAP for a partiettlar -citeut fibre Material-at> the above protocol:

[000601 lastitnntary; theFAP that is detennined.as.-desetibaherethusproVides A
Measure -for the degree tO.WhiCh the fibers in the eitruS fiber Material are available for tedispersion.
[000611 The citrus fibres in dry form according to the 8ixth aspect of the invention preferablY IttrVe A FAP Of at least 0.35 Wand more preferably Of at least 0.37 Hz The eitrat:
fibers.preferablytave.a FAP-of at most 5..0 Hz more preferably At most 3ØHz and even entire preferably at .most. 2.0 M.
[00462] Theeornposhioaof matteriodry form according to the seventh aspect of the -prewnt invention preferably hasa.PAP:ofat least 0.60 1-1z, ..;more.
preferably of at least 0..70 Az.
and even more preferably atleast0.7.4 Hi. The composition of matter preferablyhas a F.Ap of at most 5* HZ,.-1110re preferably at mostO fix and even more preferably at most 20 H. the .preferences and examples regarding the eitrusliberõ the type and amountof additiVeMbe composition of matter according to this aspect:of the invention -areas presented hereinabove for thetomposition. of matteriirdry. form tomprisingeittus fibell and an additive diStribined between said fibres aceordingtO:the -present inventiom. It is particularlypreterred that the additive is sod-6Se and that-the ratio A:17 of additive-hi citrus fiber iS-0.10.-to 1.0 and 3,0 to 1.0 by weight[000631 In an tight Aspect 111ti-pritgtiiit in ntionprwidcs cellulose fibers in dry form haying:a Self-Suspending Capacity (S.SC,) of at least 5%,.111e preferred =eellulose fibers are citrus fibers. To inventors' knowledge, no cellulose Or citrus fiberalProt.hteed hitherto had.it .$54.7: as high .as thelibers.of the invention: Preferably, the S.SC Of *dry cad* fibers is at least trYp, .more preferably at least .12%, even :more. preferably at least 15%, yet even morepreferably at lea* 17%, and most preferably at least .19%..Preferab1y,.the moisture content of dry cellulose..
fibers is:at most at wi% relativettrthe total -mass of fibers, more preferably-at most 11.:-we.4-,.
even more preferably. atmost wi%,:most preferably At most 8,wt%. TheSSt offibers may give an indication on how stable may .be a dispersion-of said:fibers in an aqueous raedia..-A
higher $SC of fibersmay.thas indicate that: anueonadispersions containing.
thereof have improved stabilities.
[000641 The'self-suspendingcapaeity" of a eitrus. fibrematerial may be.determined using.
.the following protneol:
a. providing the citrus 'fibre material in a particulate form wherein thepartieles eanpaSS:a 500 pm' sieVe; by milling thetitrus. fibre material using 'a :Waring 80.1.0W
laboratory blender e4uipped. With an SS 110 Pulverizer Stainless Steel ContainernSing its low speed :;setting.(1$000-rpm)lbr 4 plus or minus I seeOnds;':Sieving the milled material using an M200 digital shakeffitth..getsch GmbH Perinany-with:a.S.WeVt.qflOttir.n,.
500pm, .250pinand 50 urn sleA'es, whilst-shaking:flat I minute at an amplitudesetting of 60;
. .
.remillingand resievingthe particles- larger than 500 MI until they -passed the 500.11m sieve and -combining the sieved fractions b. preparing a diSpersion-Oftbe eiritis fibre MateriaktompriSing the fihreSetatitaitied in the Citrus fibre thateriat=itt aeOnceritrittiOti. of 0.1 WF.t.% bY=ttaitating The Sample using it --SilversottoVerhead mixer equipped With inEmulsor screen having round holes of .t mm.
:diameter-at:3000 rpm. for 120 seconds;
e. fining a 100 ml graded glass .measuring cylinder with 100 nal-of:said dispersion;
d. .closing the cylinder and gently turning it up anddov.in for 10 limps to ensure a proper wetting cif the citrus fiber material c, allowing the citrus fiber material townie for 241to.urs at room.
temperature -visually determining-the volume occupled by the fiber material suspension g, calculating theSSC.by-expressingthe vOl.uitteof step e. as a percentage:of the total volume:
[000651 Step a. of the above -pranced servestO facilitate efficient dispersiOn -Miring step b.
The citruslihrematerial in dry form May Conte at a-variety., of particle Sizes. Therefore, step a.
includes of the citrus fibre Maedal so as.:to. Obtain the .fibreS in the =specified particulate =
forth.; is dry Milling usinga. laboratory-Seale Waring .blender, In step t.t, ttlesitverson :overhead iniXerprefetably IS an 1,411Tovethead Mixer, f000601 The volume. occupied instep f. is Suitably=detertnined by opticalinSpectiort..Th step g.õ if forexample the volume necuPiedbY thecell. wall :materia1.
suspension is 80011,õthiS is expressed asa self-suspending capacity. SSC of 80%, [0006.7) In a: aspect, thepresent invention provides -cellulose -fibers.in dry. form haying a- yield stress (YS) of at least 2.0Pa,.-said -Y$ being:measured on an aqueousntedium containing anamount of 2.--wt% citrus fibers dispersed therein under alnw-shearstitrimt offess :Than 10000 rpm. YS:is ittc.asured on an aqueous. medium containing an. amount of Z. ot% of citrus fibers, Lexelative to thefotal.weight Odle-aqueous medium. The..
preferred cellulose fibers:are citrus fibers in a:preferred embodiment tbefibers,are dispersed undera low shear stirring, of at most.30.00 rpm. in another preferred embodiment, the fibers.aredispersed under a.
low Shear stirring of between 7000 rptnand 10000 rpitt, More preferably .about 8000. Olt and the.
YS of the dry cellulose fibers is at least .30, more preferably-atleast1.0, Most preferably at feast 0,Ø.Preferab1y, themoistureeontent Of the:dry &lb:dose fibers is at most -20 wt%.relittiVe.t to the total mass offiberS, more preferably -at itiost-12-Vt%, :even more preferably-at Most. 10 wt%, most preferably at most 8::W1N-.. The YS :may givean indication of the Boos capacity tO
hate= the viscoetaStic =properties of dispersion containing thereoti A higher YS nta-indieate that a tower atnountOf fibers may be needed to achieve certain Viseoelastie properties.
To inventore knoWledgeototelluloSe or citrus fibers produced hitherto and processed into a dispersion under theetinditiOns.presented hereinabove (e.g.:114th, fiber coneentration,..ett) had the ability:to-provide. a disperSitirt containing thereof with YS.values as high as those provided .-b$:thelprosetit ItLYCI 1100:..
[000681 in a tenth aspect, thepi*ntinventionprovideseitrus-fiberSin dryfortn, having a standardized yield stress.(Y5m) Oat least ..:2õ0 -Pa Wherein Vi*is.
measnredby a. providing.* fibers ina.parriculate form wherein.the particles can pass a 5.00 um sieve, hy-milling:the .0*w:fiber-material using a Waring$01 MG laboratory blender equipped SSII.O.Pulverizer Stainless:-Steel Container using its low speed.setting-(.t8000.
rpm) tor 4 pius or minus -1 seconds; sieving the milled material using an 'shaker frontitetsch GmbH fiermany with--aSiove set-010mm, .00p.rn,...2.501it.and 5Ø:
Am -sieves., whilst shaking for 1. minute at anamplitode setting-of 60;
remillink,I. and resieving the particles larger -than. 500 um 'until:they passed the 500. um sieveand 'Om hininglbe 'sieved. fractions;
b. ..diSpersingan turiotintathe fibers in iltirtietilate. form SO as tobbtain 300 gramss of an *Wolk, dispersion comprising 2 wt% of di Citrus fiber by weight of the dispersion, Wherein the dispersion is buffered .at H7.0;,..and-whereby the fibers art.
dispersed using n Silverson overhead inikerequipped with an Enna* screen having round holes of 1 mm diameter at 3000 rpm for 120 seconds; .and c. using a parallel plate rheorneter determining theshear storage modulus-kr-of the resultant dispersion asallinction of the:strain:percentage. and establishing -the YS* from ibp.inaxiittptu-ofthe shear stortigemodulits.0' versus the strain percentages, [00069] .Step a. a-tea-hove-protocol for thedetertninationiofthe YS ik serves to facilitate efficient t.lispersion.:ditring step b.-The citrus fiber iii-dry form may:come at a variety of particle.
sizes. Therefore; step a. includes milling Of the eitrua-fiber so .3.S.
toobtain:the fibers:in the specified particulate form. Suitablemi llingis provided by dry .m Ming using a laboratory,scale Waring blender. The buffered dispersion. or step b, may be prepared'using any suitahle.buffer.
system. Preferably; a phosphate-based bufferis used in stepe. the SilverSon overhead mixer preferably is an lARTOverhead mixer. G.7 is Measured using any suitable parallel .plate rbetimeter,õibt example an .ARG2- rheometer of TA Instruments. 0' is measured at various. strain benriderstood by the !Skilled person A preferred way of establishing the:YS*
is by folloWing the protocol in the way deeribed below, The above protocol and the Examples provide methods of measuring the Y$4,. However,. the .YS* May ablo be determined by.

different prot6Col, as long as that protocol - would kadlo the Samephysical 'result:, i.e. it Would yield theSameYS*--Ibt.aparticular drycitrtis- fiber preparation as theabOVe protocol.
[000701 'The citrus fibres according to the tenth aspeet.eftheinveritibit preferably hinie a.
YS*- Mit leaSt :2 Pa, More preferably' at least 3 PA,. fA`011 More preferably at -feast 4 Pa and still morepreferably,at 104-44: Pa, The Citrus fibers preferably have &atulardized.yielrf stress of up tp.50 Pa, and -morepreferably of Op to 20 ThuS Particularlypreftvred that the citrus fibers in .dry formõhave-a:standardized yield -stress of between 2 Pa and 50 Pkmorepreferably between 4: Pa And 20 r4.
[owl cjoyerith aspect, the present 111VpntiOn prpvides a composition of matter in-dryfortneompriSing citrus fibers and an additive distributed between said fibers, said.
composition .having a.transversereiaxation factor rgev-I.:as measured .by nuclear magnetic resonaneerNMR1..ofatteasti 0.10, Preferably, the Re 'valueotsaid composition is at least 0.75merepreferably at least kW: even-Inore preferably atieag OS, most .preferably atioast 0,04. Preferably, theinoistureeontent.of said composition' is-04110st 20:wt%
relative -to thetotal.
mawoffibers, Morepreferablyet most f2-Wite/ii, eVtn.:M.Ore-pireforibly at mOst 10 WA%, itiOst preferablyahnost 8 vit%. Preferred examples,atidpreferred attiotintS Of the additivetts.*ellas Suitable Al' ratios are -presented aboveand will not berept ated herein.
[000721 In a.
twelfth. aspect, the .present invent ion provides a composition Of matter in 'dry' -tbren comprising Chins fibers and An additive distributed between Said 'fibers', Said .composition having, aself-su.spending capacity (SSPolit least !9%...PreferablYõ:The.S$C. -ofthecorripoSition:
is at least more preferably at-least even more preferablyat least MS, yet even more preferablyat least 19%, and most preferablyat least 21%. Preferably, the moisture content-of said composition is..at most20 -wtSõrelative.to The totalmass of fibers, more preferablyat:most 'Zweig-. even morepreferably at most 10 wt* most preferablyat most # NiftN.
Preferred examples and.preferred amounts of the. additive:as well as sultableATratios are pmented.
above and will not be repeatedibcrein.
-1000731 In an thirteenth aspect, the pmsent inventiOnprovides atviriposition,ofmatter in dry formeemprising citrus fibers:and an additivodiktributed between said Abets, said composition having a yield stress. (YS) of at least 10 Pa, said ys being measured'on an aqueous medium !obtained by dispersingan attic:lima-said composition -therein under a low shear Stirring:
of less than 10000 rpm to obtain atints fibers' tontentration of YS
iStleasured On an aqueous medium containing an amount of 2 wt% of citrus fibers, Le;- retatiVe to the total weight Of the aqueous Medium: Preferably, the YS is at least 3 0 Pa, More preferablYatleast 5.0 PA, evert mote preferably at. lea* 8;0 Pk, yet even more preferably at. leaSt 10.0=Pa, yet even more .preferably at least MO Pa, most preferably - at leaSi 14.0 Pa, Preferably, the moisture eontent of .20 said composition is at most 20 wt%.telatiVetOthetotal mass of fibers; tnOit preferably attoOst 12 wt%,. even more preferably:at-M-6st 10 wt%, most preferahlytt most 8. wti.
Preferred examples.and preferred amount Of the additive4s. well as snitable:-.AT ratios ati.!:- presented aboveand Will not be repeated [000741 In a tburteenth aspeet, the present inveritionproVideS a COmpositiOn Of matter in -dry forth Comprising CA* fibers and an additiVedistributed between said fibers said:
composition haying,.:baVing.a standardixed yield .stress (ys*). ofatleast. 2.0 Pa wherein the 'VS*, is:nteasuredby --proyitlipg the. composition in apartictilatefonn wherein-thepartieles:.can pass 4 500 tim siem by milling the am-fiber-material usinga:Waring 8t:00a laboratory blender equipped with an -S$11.0 .p.iftvexi4xu-S tajp)igss Steel. Container using its low -speed setting (18000-rpm) for 4-plus. or minus 1 seeondg.sieving the milled ataterialusingart A$200.
slutkerfrom.Retsch dmbli Germany with a:sieve set-of I (nom, -500gmõ:250001.
and-5.0 urn sieves,-whitstishaking for-1.-ntinutc.at.an aft mitudesettingoffik-remilling --and-resieving thepartintes larger than 500-.nit until they passed the 5.00 im sieve and Combining the sieved fractions;
b: dispersing an ItinOuntelthe composition in .particulateforni so as to obtain -3%)- grams of an aqueouadispersion.compriaing,2 wt% of dry eitinS fiber by weight Ofthe dispersion, whereintheõdispersion is buffered.* PH 7 0, and Whereby the fibers are diSpersed.OSinta-Silverson overhead Mixer- equipped With in .Einulsor screen having round holes of .t diameterat 3000 rpm for 10 seconds; and c. using a parallel plate rhemneterdetermining.the shear storage modulus, ar of the resultant:diSpersion asafnuction of the strain percentage and establishing the .yield stress from the maximum of the:shear:storage modulus. (V -versus the strain percentages.
1000751 Step a. of the above protocol for-thedetemination-of the YS' serves to facilitate efficient dispersion duringatep b.-The composition of matter in dry-form may:come at a variety of partieleslies..TherefOrey. step 4, includes: milling Odle composition so as to obtain .the composition in thespecified: particulate form. Suitable- milling IS provided bydrymillingosinik A
laboratory-scale Waring blender; The buffered dispersion ofstep bArto be prepared using Any suitable butler system.. Preferably, a phOsphate-based buffer is used. In stepc:-..the.Silverson overhead Mixer preferably- is ad TART overhead mixer. .G is Measured using an'Suitable parallel.platfl.theortiet&Obr example an ARG2theorneter of TA histrUmerits.-G.'`-iS Measured at .arlotts Strain levels as Will be .underStOod by the skilled perSon...Ai.prehirred way Of establishing the-Y-S!!! 4-0$ foltoivingth.epii.4(idol in the ay described help*, The above prOtOe.0 and the ..ExaMplesproviide mett4)ds of measuring the YS*...floweVer; the Y$'"fnay also: he determined by a.different pnatoCOLas long as thatpthtocol would lead to the same physical result, Le. it would yield theSameYS*for. a particular dryeitruS fiber preparation as the above protocol.
[000761 'The composition of num* hi thy form according to the fourteenth aspect of the invention preferably.has. a. YS* ()fat PeaSt.2-.Pa4 more preferablyat least:-3 Pa, even more preferably nt Watt. 4.= Pa and stilt ritOrt preferably at least: +.5.114, The compoiftiOn of mat* in dry forth PreferablY has a standardized YieldstresS Y5* of 5.0 Pa, and morepreferabIY:of op to. 20 Pa.. Thus ftisparticulariy..preferred that the compositionOf matter indry form .has a standardizedyield stress VS.* 'of :between 2 Pa and 50 Pa more preferably between 4 Pa and 20.
Pd. The preferences andexamples-regindingthe citrus fiber, thetypeand amount of.addifive in.
the compositionof matter according-to this a..speetoftbeinyentionareas presented hereinaboye for fhecomposition of matter-in dry farm comprising citrus fibers, and an additive distributed between .saitlibers according:to* -presentinvention.
-100077] :in a. fifteenth aspect thepresent inventitm:providon dispersion comprisinzeitrus:
fibers dispersed in annqueous medium, said dispersion. having a (.1 value of at least-50 Pnwhen measured at a fiber COne.entratiOn of 2 wt%. re! ative.:to the tetal mass of thedispeitinn.
Preferably,- Said G' is. at least 100 Pa, more preferably.atleaSt 150 Pa, even more preferably at least 200 Pa, yet even More preferably at- teaSt:250 Pa, rifest preferablyat leaSt:350 Pa.
Preferably, said dispersion has stresSlYS) of at lea5t-2,0Paitrufrepreferahly at. least 3.0 -Pa, even-in-tire 'preferably at least 5:0Pa9 yet even more preferably at least 8,0Pa, yet. even More ..preferably at least 10.0 Pa, yet even Morepreferably at least 121) Pa; most preferably it least 14.0 'Pa: Examples of dispersions *Mc withotn.Jimitation suspensions, emulsions, foams and the like. Illecitrus.fibers in the dispersion may hayeit Brownian motion or they may be fixed at an interface.presentin the aqueowinedium.
[0007811 Ina sixteenth as-1feet,-* present invention provides a methodfOrmatufficturing the inventive fibers and/or eompositions-comprising the steps of:
a. -Homogenizing anaqueous:siurryota.source of citrus -fibers to Obtain an aqueous slurry of citrus fibers;.
b. Contacting theaqueous slurry of citrus fibersith.an organic solvent to obtain a Precipitate Phase and a liquid- Phase; Wile-relit The. PreciPitaWIS. in. the ,forirl ofgranules;
e. Separating Said precipitate phase fitful the liquidphaSe to .obtain-asettiktry eitrus:fiber cake havinga dry substance-content Of at least 1 0 WM relative.thithe mass Of Said cake;
d. Comminuting said cake to obtain grains .emitainitikeitruk fibers; and .mikirtii, Said:101ns-with an additiVelo obtain tisetni-drytomposition tompriSing (In* fibera and an additive; and.

e..Desolventizingandiordaydrating said semi-dry coMpOsition to obtain a dry composition Containingeltrusfibers andan additive, and .having a moisture contentot7-preferably beloW 211 Vrt% relative .to. the. total weight of the fibers.
[00079] It is diffictilt to prepare adiycornpoSition tontaining.aitiS
fiberswithont affecting the eampOSifiOri'a diSpersibility in an aqueouti-MOia... This.
difficulty IS attributed to many factors (ColleetivelY referred to in literature as"hornificationlaugh as the formation of .hydrogen. bonds and/or-lactorie bridges betweenthe fibers, HOrnifieation typically reduces the available free7surface area of the fibers andlor strengthens the iinkagehetwern the fibers, which.
in turn may reduce the capricitrof.the fibers .to absorb liquid and thus.io.disperse. compositions containing horn-010d dry citrus - fibers either cannot be dispersed into an -aqueous-medium, -e.g.
water,. a. water solution or a. water suspension, or they can be-dispersed only by using. high or 140a-high shear Mixing, 10001 The method oftheinvention :succeeded however in producing dry -compositions 'wherein thehornifieatitin.ofthecitrus fibers' was largely prevented.. Without being bound to any .theory the inventors believe ttiatany Of the Re, .issc and.YS.a well as the reduced-deviatiOrWof STDEV from MAX characteristic to the inventive-fibers-and inventive coMpositiensinay indicate a reduced homincation Of Said fibers.
[00081 The method of the invention .(the invtmtive method), containaastep of -liOntogenizing:an AqUOItS. Slurry Of a source of clans .(Ibett e*Souree SlorrY").. 'Mc source of citrus to**. maybe citrus peel,:eitrus-Pulp, citrusragor-combinationS-thereot:
The source:of citrus fibers maybe a by-product obtained during the pectin extraction.
process.. Preferablyõ:the source-of the citrus fibers is. citrus peel onorepreferably is depectinii0 citrus peel, Said 'source-:slurry preferably comprises a dry substance -content of at least.2w-N,Anore preferably atleast 3 wt:04,...more preferably at least. 4 wrii. Preferably saiddrysubstaneecontent ofsaldsource shiny.
-is at most tO w%, more preferably at m.ost.11-10,1,, most. preferablyatmost wt%.
1:000821 The homogenization of the source Slurry. may be carried, out with ammtber of.
possible -methods including, but not limited to,. high shear treatment,.
pressure homogenization, eavitation,exploSiort,: pressureinerease and pressuredropireatments, colloidal milling; intensive.
blending, extrusion, ultrasonic treatmentõAnd combinations thereof_ [0008:31 Inapreferred ettitodittent,Jhe homogertiiiition Of the source slintyisa. pressure-homogenizatientreatment which maybe carried out with a pressure hOmogenizer.
Pressure homogenizers typically cortiptige a reciprocating plunger or piston-type pump together With .a hoMogenizing.valve assembly affixed to the-dkcharge end Of the homogenizer :
Suitable pressure homogenizers include high pressure .homogenizers manufactured by G.PV
Niro .S.:04.1' of Pttima (Italy), such ts the NS Series, or the homogenizers of the Ontlin atid.;Rannie twries.

maaufachtred -by-APV- Corporation A...Everett, MassachusettS.(1.1S).. Daring thepreSsure hontouenizationõ the-sinter:at slurry- is subjected to high ShearrateS as. the result Of cavitationand turbulence eillbets:- These effects: are created by thesoureeslurry eotering:a homogenizing Valve:
asSeinbly=Whiehis. pert Of a pump section of thehoinbgenizerat a. high pressure. (Arid low Velocity). Suitable pressures tot the inventive method are from .50 bar to 2000 bar more .preferably between 100 bar and I 000-bar. While not being- hound to any theory, it is. believed that the .hoinogenization oases disruptions of the source of eitrus fibers and its disintegration into the fibrous component.
[0.004) Depending on the particalar pressure selected. for thepressurehomouenization, aridthe flow rate ofthesogiveslarry through the homogenizer, the source *wry may be homogenized by one pass.throtigh the homogenizer or by multiple passes. in eineembodinient, the source slim) 1$ homogenized by a single pass through homogertizmiltra:single pass homogenization, the pressure used ispreferably from 300 bars to 1000 bars.
more preferably from 400 bars to 900 bars, even more preferably from 500 barsto800 bars. in another-preferred embodiment, the settee:slurry is homogenized by Multiple passes thrOtighthe homogenizer, preferably at:least:2 pasSeS, mere preferably at least:Ipassa.thrting#the homogenizer. hi 4 Multi-pass homogenizatiOn; the pressure use.d is typically lower torapareikto a.Single-pass.
homogenization and preferably -from .100 kittei. to 600 bat* More preferably from 200 bars to .500 bars, even more preferably front :300.-bars16400 bars,:
f0008.51 The result of the homogenization Step -is anaqueonS.Slurry of chrits..fibers ("fiber slurry") comprising a dry Substance content of fibers in essentially the same atitount as the sourceslarry. Said-fiber slurry is then contacted with an organic solvent.
Said organic solvent .should preferably bc. polar and water-miscibletobetter facilitate water removal, Elamples of suitable organic solventS.--wbich :11reppfar.apd water-iniseihleinclude;
withott.t.
.aletiltols-such as -methanol, ethanol, propanol, isopropanot and batanol.
Ethanol and isopropanol are preferred organic solvents;:isopropanol is the: most pmferre41- prganic solve* for use in -the.
inventiVernethod.. The organic. solvent can be used init$ 100%pure. form or may be a mixture:of org Solvents:. The organic solvent can also be used asamigure of the organic :solvent: and 'water, hereinafter referred to as an aqueous solvent solution.
Theconcentrationof organic.
solvent in SaidaeueousSOlvent solution is preferably from about: .60 Wt% to about 100 wt%
relativeldthe total weight Of Said solution, more preferably between 70 wt%
and 95. Wt%, most pri.iferably between 80 Wt% and 90. wt%..-Ingeneral;lower c.oneentrations.ofthe.orgartie solVent.
are Suitable to remove. Water and Water-Soluble:CoMponeritS whereas increasing the concentration of said organit solvent also hcips in removing oil oil-sOlubjecom laments- if=
-desired In one embodiment, an organic solvent Mange containing a .non-polar organic (NPO) 00-$Olveatand the Orgattiesolvent.orthe aqueOuSselverit Solution is used to theinventiVe Method. The utifiitition ofthe 'organic Solvent Mikturetrtay irnprove fordittuttple the recoVery-Of components in thetittus pulp, Exalt*lesof Snitablels1POto.,solventS
without limitation :ethyl apetateõmethyt ethyl ketoiiacetonc. bekane.methyt isotaiWketinte iand toluene. The NPO co-SelventS are preferably added in amounts of up t6-20%telative to the total amount of organic solvent inixtute.
[0008.0) The fiber slurry is contacted -With:1hp organic solvent preferably in a tatio Slurry:SOlyent- of at most 1:11:, more prekrably at :most 1 (iõor most preferably at most 1:4.
Preferably sairititio is at least I :05,. more preferably at least I :1 , most preferablyatieast 1f2.
Preferably, said fiber slurry is. contacted with:the organiesolvent for at least lOninutes, more prefetahly:for at least 20. minutes,. most preferably for at lcast:30tninates.
Preferably, said slurry is contacted with the organicsolvent Total most several hours, inorepreferahlykrat-most 2 hours, most preferably for almost.. I lto.ur.
[000871 According to.the invention, said fiber slurry:Is. contacted with said organic .stilvent WI 'Obtain a precipitate phase and a liquiciphase. The inventors.
observed thatduring.
contacting the organic :Solvent with the fibers Awry; the:Tibet slurry releases at least part of its water content into the organic solvent Which in turn causes :the citruS
fibers: to precipitate. By ithase. is herein understood a phasetontaining the 'majority :of the .eitrus.fibet*.eig,-motethrin;80% of the total amount of fibers, preferably more than 90%, MOST -prefriably more than %N and also Containing organic solvent : and water: theprecipitate phase:
usually settles clue to gravity fOrces: The precipitate phasetypically has a. Solid ¨or a gel-likeappearance, icit essentially -maintains its shape when placed on a. supporting .surface.
1).y"/10.4(1p4coe is herem.
understood a phase containing organic-solvent and water; The:liquid -phase.
may also contain some citrus fibers which 40 not precipitate; According to: the ibveritiop,the precipitate phase is .ip.the. form Pfgranules, preferably, millimeter-sizeuranalps.. Preferred granule sizes are between 1 nun and 100 mm,. more preferably between 5 min and 50 mm. By tlitesizeof a granule is herein understood. the biggest dimension of said granale The. formation of the precipitate phase Into granules may be achieved forexample by blinging the fiber slurry -under agitation into a.
container containing:the organic solvent or by.pouring said slurry in the.
organic. solVern.
amount Of agitation typically dictateS-the site of theforened-granales, it.Was observed that by forming granuleS, the subsequent water removal from: Said granuleS
igfacilitated: Without being bound to any theory, itig believed thatthe. tbrtriatioitof grannies also aids-in preserving and/or increasingthe free surface area of thetitrug fibers .available .for Water binding and may also :-.4vOid a collapse Of 00 fiber*

[000881 The precipitatephasels subsequently separated from the liquid phase to obtain -a semi-dry. citrus fibers cake (fiber Cake"). Said separation can be- athieVed using known-methods such as Centrifugation, filtration, evaporation' and combinations thereof.
[000891 To increase the dry substance content, stepsh) and .e). of theinventiVe iiiethOd Can-tu repeated at least one titne,preferablybetbre-Carryint OM Step d).. The fiber Cake can also he subjected to an extraction step: Apreferred.exfractionmethod is pressing, e.g.
with a normal press. A screw pres.sor an.extruiler.- A:more Preferred extractionmetbod is..pressure filtration .using A volume chamber filter press.ora. membrane filter press;
pressuiv:liiters.beingsOld for -example,by-13K$ -$onthofen, DE Two7sided 'liquid removal :Issecommended for the pressure.
= Oration since more :filteringarealsgvailahle. per volume.orthe fiber cake:
= [000901 The Ober eake issem.Wryõ.õ1...e. ithas a dry substance content ofpreferablyat least l0-wt% more preferably. of at le.00.1.5 wt%, or most preferably of at-least:2Q
ut% relativetothe maw of said cake: Preferably, said cake hasaliquid7content.ofat most:50,-wt%,.more :preferably at VitIst most proem*. at:most 30 wt% relative to the total massof said cake: The:
liqUid.-typitallytontainsorganie solvent andWatet, [000911 ItraCCOrdance-With .theinVention, the :fibereake is Cbirlit intitedlo-A4MAiti grains.
containing citrus' fibers rliber grains"), Said grains preferably having a diameter rifat Most .100 tinn, more preferably .at most 50 mm, even more preikrably-at most 30,mink.yeteVert'more preferably At most 10 iptu,.yet even more preferably at most 5 rnin-, most,.prgferably at Most 3 mtn. With, "graindianieter" is herein understood the largest dimension of thegrain. Thediameter may. be determined using .a mieroSeope equipped with g,raticuleõCinters may he used to.cut the fiber eakeinto. grains. Alternatively, the fiber cake can subjected tomilling and/or grinding in order to form it into grains. Examples -of suitable means tocorturtinute the fiber cake Maude without limitationa cutter mill, ahainmer mill, a pip mill, ajetmill:.and:rhe like.
[000921 The fiber -grains are mixed withan additive to obtain a semi-dry composition compriSihr citrus fibers and the: additive-Examples of suitable additives as well as preferred chokes 'amgiVen above and will not be repeated herein...Mixing the 'fiber grains With the additive on he effected with knownmeansinõ the art,.examples-thereofinoludingoithout :limitation a malaxer, A transport serew,...an air-stream agitation mixer, a paddle mixeri..a Zsinixer, a turable Mixer, A high Speed paddle mikerõapower blender and the like:: The additive maybe.
provided in a Solid-form or in solution. Preferably, the additive iS 01*i:fled ina.tolid form; more preferably as a nowdte, oven more preferably as a:powder having:Ai average partielesize-('APS-7):Of between '100 'And.500:tirt, More preferably betWeen 150 and 300-prn;'the APS Can be determined: by.ASTIvr C136706.
.26 [00093] The semi-dry composition issubjected to a desolventizing and/or dehydrating step-Wherein the organic solvent Ara/or:the .water are extracted from said rempoSition.õ
Preferably, the inventive' method contains bothsteps of degobtentizing and dehydration:It:Was:
surprisingly observed that during the organiesolVent -and/or :Water extraction4he hernification of 00S-fibers WaS largely prevented Without being bOund to antheory,: the invotitOrg attributed-the tedoced.hornifiCation to the .careful pre-processing of the composition prior to said p)nractiortas detailed in steps a) 03 Opf theinventivemeth4 [00094] Desol vernisation and dehydration ofsaid composition can be carried out with a desolventizer which removes organic solVent:andlot water from the .corapositiOu and may also:
enable the mimic solvent to, be reclaimed** future use. Desolventizing also ensures that the.
obtained dry composition is safe formillingand commercial: use. the desolvept4er can employ -indirect heat to remove the orgapto;solvent from the; composition.; the advantageof using said indireetheat is that significant amounts of OrgardOsolvents can be oxtractott.Also,.-direct heat on:he:provided fOr.dryitig,.e.g. by:providing-hot* from flash dryers or fluidized bed dryers.
Direct steam may be eittplOyed, if desired,. to retnOve any- trace amounts of 'organic solvent yernainingin the composition. Vapors ftein:the desolventizer preferably are recovered and fed to.
:a Still to reclaim at least it portion of the organic-solvent.
[000951 Retention tiftt6, for the desolveritizing dehydrating step may:Vary.oVer *We *10 but Can be about 5 minutes or legs. Suitable temperatures at which Said -desolventizing and dehydrafing.itep is 000 out dependon such factors as the type of organic sol,nt and Most often ranges from about 4 C to about 85!T at annosPherk pressure Temperatures can be appropriately Increased or decreased for operation under supra, or :sub.-atmospherie pressures. Optionally, techniques :;such as ultrasound amused for-enhancing efficiency .of-titedesolventizing and dehydrating. By-trutintaininga elosedsystem, solvent lows can be minimized. Preferably, at least about 70 wteA of the organic arilyent is recovered and reused.
1000961 Dehydration ca be affected wit] known means in the.
art,..e.xampl.e.s thereof including-without limitation paddle driers; fluidi2ed bed Mem:stirred vat uum.driers, drum driers, plate driers,. belt driers,-.microwave,drieN and theflikeõ Preferably, the dehydration temperature is at most :100 C, more .prefet-ahly at most80 'C,..most preferably at-most 6041C.:
Preferably, the elehydrationleitiperatureiS at least 30 C., more. Preferably at leak 404C, most .preferably at least 30c, . POW) The desolvetnizingand/ior dehydrating step are carried patio obtain a dry composition comprising citrus fibers. and. an. additi.v.e.,õ said:dry composition having.amoisture-enntent at at most 20 wt% relative to the total of the fibers, preferably at most more preferably at Most 12: wt%, even more preferably attunst 10 wt%, inOstpreferably at most 8 wt%, [000981 :Optionally, the Method of the invention further comprises a Steptfriiinoving said.
additive tindlortiaSsifying.the dry corn positionto obtain thedesired partielesikeitild/or packing the -dry eompeSitiOnõ
[00099] inapreferred einbodi Mein, theinYentiVe Method comprises a claSsifiration step = Ofthe dry composition which may improve thehomotreneity of the.powder, narrow particle size.
distribution and inaprovedegree.ofrehydration, Classification may be ratriedout using either a.
static or dynamic- clasSifier, The inventive method may- further comprise it packaging step of -the dry composition.
[0001001 in apotherprefetred embodiment, the:additivels extracted from the dried and/or classified composition as Obtained at steps f) and/or g), respectively to obtain dry citrus fiber.
:TO aid in the extraction a the addit e.prefebiy, an additive is: used that has a boiling point of less than the degradation-temperature-of the -citrus-fibers.. The extraction may be performed by washing the additive Withu suitable-Savent other than water. The-extraction is preferably performed by.subjettingtaid edittpetitiOn to anextractiOn ternperatere between the boiling point of the additive and the degradation' temperature .of the citrus fibers.,atul allowing the additiveto evaporate; preferably the &Oblation is Carried outtitider Vatutim. Preferably, said additive has a hailing point Offat most 250: C., .More.:preferablyat most 200 most 'preferably at most 150 C. The boiling points of various.materials are liatedin theCK Handbook of C.hetrtiStry and Physics or alternatively, A.$114. DI 120 may be used to determine said boiling point, Preferably the extraction. temperature is between 100 and.10.0 Cmore preferably between.
too ar.o.:25.0 most preferably between 1.00 and 200 C. Examples of additives. having such reduced boiling points include IOW molecular weight pOlyols,-e.g. pillyetherpOlyOlS, ethyleneglYeOis, and the:
like. By kiW inolecularweight is herein understOodart.Mw of between 50 and :500.. The use.of such extractable additives enables the Manufacturitigof the inventive fibers.
Alternatively, dry citrus fibers -May be:ObtainedWith-the inVentiVe method by skipping in Step d) the addition Of the i-additive by inixing,-DryeelloloSe fibers may 'also. be Obtained with the method of the invention.
:by choosing an appropriate source of cellulose fibers to he processed,.
f.0001011 l'he dry -eompositio.n comprising the citrus :fihers.andthe additive is preferably .milled and cia.s.sified to obtain a powder having an average particlexizeormfetably at least 50 urn morepreferably atleast.1501:ton, most preferably at least 250 tutt_Preferably.said .avemgepartielesize is at most:2000 um.,:morepreferably at most 1.000 turt, most-preferably at most 500 pm, Said. average:. particle size may be .determirtedbyASTM:
C13,.6416.
.28 [0001021 in a seventeenth aspect, the invention relates to a. compOSition of niatteriti .dry form obtainable by the method lbr manufacturing the composition.aceording to the Sixteenth aspect of thepreSent invention.
[0001011 The inVontion. will be further detailed in. the followingexempiary embodiments, without:being however limited thereto, [000104] in a Ark: embodiment, the inventive. composition -of matter dryfortn comprises:
*Ms fibers and an additive -distributed between said fibers, :wherein said cOmpositiOn'has transverse Niaxation factor (lt;i*). of at least 0.10õrnore preferably of least 0.75, more -preferably of at least 0.85, most preferably ofat least 0.99, ,wiwrein when dispersing said composition with a low shear stirring of lesslhart10000 rpm in an aqueous medium to: a fiber concentration (.)Lf 2 wtS, the Obtained. dispersion:has a G' value of at least 50 .Pa. Preferably, the dispersion isearried outwit a low shear stirring of:at-most-8W rpm, more preferably At most:500 'rpm, mostproferably at most. 000 rpm. I.Preferitbly, the A:IF ratio of the. compositioo = is between and 10:1 by-weight, more preferably between Ø1:1 and 9:1 by weight, most preferably between and 8:1 by weight. Pre&rably,- tbetitrUS fibers did not undergo any.
substantial chemical MOdifietitiOn. Preferably, the additive is chosen front the group consisting of fructose, manneSe, galaetoSe, glutose4alo* guloSe, -acne, Arose; idose, arabinose..xyloStt lykOse, riboae, siterbSei maltoSe, -lactose; glycerol; .sorbitelõ'starth .and combinations thereof:-[0001051 itt-trscodriii:eMbOdituditti:the inventive composition of Matter in dry fbrin-coinPriSesieitrusi.:fibers and an additive distributed.betwemsai0 fibers,õwhereinsaid composition has.a)SSC of at least 9140nd A transverse relaxation factor (t?) Oat least-0.7Ø Preferably, the --5:fi( of the :composition is atleast 13Piii, more preferably at feast I 5,0.
even moropreferably at least 1.7%, yet even more priforablyM *AM 19%, and most preferably at le* 21%.
Preferably, the Ita* vatwotsAW composition is at least: 0.75, more preferably at least 0.80, even more = preferably at least 0.85; mostprefitrably at least 0.90. Preferably the ..A:f ratio of the is between- 01;1 :and.:10:1 .by weightmore preferably between 0.1-A and 9:1 by veit.doõ.most.preferablybetween 0.4:1 and 8:1 by weight,. Preferably;
theeitrus fibers did not -undergo any substantial thernicantodification .Preferably; the additive.
is:chosen from.. the-group:
consisting fru. etose,:matmoseõitalaetose, glucose, taloseõgulose, a lose,altro.se, !dose,.
arabinose,.--XylOSe lyxoSeribrise, siterOst, maltose, lactose, glycerol, Sorbitol, starch and cortibitititions thereof.
[000106] in :athird embodithent, the citrus fibers of the invention have a transverse:
relaxation faCtorrit?").-AS MeaSuredbknuelear Magnetic resonake "NMR") Of at least 0.7-at4aSelf-suspending capacity- (SSC) of Watt -9%. Preferably, the It? Value Of Said dry cellulose fibers. is at least 0.9, even more:Preferably at least Li, and most preferably at ktist-.1.2õ
.29 Prekrably,:the-SfiC of Meaty. telltilost fibersiS at least 12,-even attire preferably. -atleaSt 15, yet even more preferablYat least 17 and most preferably at least19: -Preferably7.the moisture content .of thedry citrus fibers: ht-itt moSt.20.0"-relative to the total mass of fibers,:. more preferably at theSt 12 wt%,i Mien nabrepreferably at Most 1.0 AVt%, most preferably at -triest 8wf%.
f 0001071 In a fourth embodiment the inVentiOn relateS.to citrus fibers in dry -form having A
storage modules KiFI of* least 50 Oitt 6' 'being measured on an aqueous medium containing an amount of 2 wt% eitrus. fibers :dispersed therein nndera low-Shear stirring oriess.
than 10000 rpm, said fibers preferably havinga transverse relaxation factor ("Rik"): as measured by -nuclear magnetic resonance ("NM") of at least 045.õ.sald fiherspreferablyintying a self-suspending capacity (S.LS.C.)of at least 5%, said fibers preferably having a.yield-stress (Y:$)::ofat least 2.0 Pa, said Y,S!beina measured on an aqueous medium- containing an amountot2 wt%
citrus fibersdispersed therein under a low-shear stirring. of-less:Than 10000 rpm. Preferably, said G is.ativast. 75 pa, more -preferably at least 1.00 Pa, even more preferably at least 125...Pa, yet:
even more preferably atleast 150 Pa, moscpreferably at least 170 PA.
=Preferablyohe stitring.
Used- teachievethe dispersion-Of said citrus-4%0S in theaqueOus medium is at most 8000 rpm, morepreferably at most 5000rpm, it Ost-prefetabiyartioSt 30004m. Preferably, said citrus 'fibers Contain an amounrof water of at most 12 wt%, Mrite preferably .atirtibst-10 wt%, or most preferably At. most 8 wt%, Preferred ranges forlte!, SSC and YS are piOdtik,d herein above where the thud, fourth and fifth aspects of the 'Mention, respeetivelyõ-aro:
detailed and dl not :he further repeated hereinõ
10001081- Ina .fitlb :embodiment, the invention relates to a composition of matter in diy form comprising citrus fibers and an additive...distributed between .said fibers, said composition has mg a storage modulus:WI-of-at least 51:k Pe, said 6 being measpred on an aqueous medium obtained by dispersingan.amount of composition *rein tinder a low shear-stirring of less than 10000 rpm to Obtninacitrus fibers' concentration-0.2 wtS relative to the total ampogtof the mueoustnedium,..said composition preferably having-a transverse relaxation factor -("gei`"):
as measured by nuclear triagnetiaxesonanco Mr) of at least-100,.said composition preferably having A self-suspending. capacity (S SC) ()fat least 9%,. said composition preferably having a-yield stress (YS)-ofat-least 20P.a, said yti being measured on. an aqueous. medium Obtained by dispersing anattiOunt of said COmposition therein under a le-Wt.:shear stirring Of less .thanI0000 min in obtain atitritSfihers' concentration of 2 WM, Preferablyilbe composition.
Contains .an -amount:Of water of at most.1.2 wt!.%$.i more preferably at.most 1.Owt%, Or most preferably at most 8 wt* Preferably,. the composition has an additivefiber (A:T):ratio.of 'between 0011 0 and 10 0 1 0 by Weight, .mOrt preferably between 0;1 ;1Ø-tind 9;0 0 by 'weight, most preferably between 0.4:1:0 and 8.0:1.0 by weight Preferably, the additiVeis chosen - &Oro thezroup eonsisting of glucose, sucrose. glycerol and Sorhitolõ
Preferred ranges. for G%R2*.,-SSC and YS are presented herein above where the Setondõsixtk-Seventh and eighth aspects of the invention, respeetiVely., are detailed and will not hefurther repeated herein:
1:000.109.1 It was observed that the. inventive Compositions have an Optimal ViSeothiStic =
fittetuationS.Of einripOSitionS? Viseoelattie behttiior,:: The ability of the inventiVecoMpositiOnSto smoothen out vist!oelastie fluctuations May enable a more reliahle processing dieted which in nap may lead to optimal quality pf various .produets containing said composition, e,g.,:food, :teed,- personal care and phartnaceutiCal products.
. POO 101 The inventive :-fibers and the inventive .compositionstwe suitably used in the -production of a. large variety of food compositions. Examples of food compositions. comprising thereof, to whieh the invention relates, include.: luxury ;drinks,...such as:coffee, black lea,.
.powdered green tea, cocoa, arlzukVbeansoup,. juice, soya-bean juice, -etc.onilk-component4.
con tainingdrinksõ such as raw milk, processed inilkJacticaciti beverages;
'etc.: a variety of drinks including nutritiOn-eririched,driiiitrouebas ealcium-fitified drinks and the like and dietary fiber-eOntaining drinks, etc.; deiryprOduets, -melt as butter, Cheese, yogurt; coffee whitener, whipping Crean', custard orearni custard pudding, etc.; iccdproducts such as ice cream, Soft cream, lacto-ice, ice Milk, sherbet., frozeng.urt, -etc.; processed fatfood.products, such as mayontiaWmargarineõ spread, Shorteniniti, ete:;. soaps; stews;.seasonings-stieh sauce, TARE,, (seasoning Satiee), 4reSSinks, etc.; avariety of page Cenditnents, represented by kneaded mustard; a variety of t1lings typified by. jam andllottr paSte;..-a variety, or .gel ot paste-like food ..rMiducts including red bean-jam, jay, and foods for swallowing impaired people; food products :containing cereals as die.tnain C0111.1)000111, :such as bread,nood les,.
pasta, pizza pie, corn flake, -etc.;.:Japanese, US and European cakes., such as candy, -cookie, biscuit, het cake,. chocolate, ricv cake, etc.:; kneaded mewine products:represented by.a holletlish.vake, a fisb cake,.tc.; live-stock products represented .by ham, sausage, hamburger steak, etc.; daily dishes such. as cream croquette, paste for Chinese tbocts, gratin, dumpling, 'etc.; foods of delitateilavor, such as salted fish guts, a vegetable pickled in. sake lee, etc4.1i1uid diets such as. tube feeding litiuidlood, etc.;
supplements; and perfOods. Thesefoodproducts are all encompassed within the present -.'invention, regardless of any difference.' in their forinrand processing operation at. the titneof preparation, as seeifin retort foods, fro zen foods nrieroWave foOdS,etc:
[0001111 The invention also provides a food eonipoSitionin dry. form, comprising the -Owns fihretiecOrdingto the invention and/or the:compoSition of matter in dry forth. according:hi 'the -invention, SOCK a food composition in dry form preferably cOmpriSetta=COMptisition of 'matter in dry=form, wherein said Composition of lman& omoris4- citrus fibreS
and an additive 3.1 distributed between said fibres. It kpar.tiettlarlypreferreddiattheadditiVe is Sucrose and that the ratio A:17 of additive to citrus fibre is.-0.10te 1.0 and hyweight.
[0001 121 It was Surprisingly found that-the- citruslibreSin dry forin of the present invention and the compasitionin -dry form- cornpriSingeitruS fibres and an additive Of thepresent invention.
can be readily dispersed in an aqueOus niedinnt.- Therefore, the* Oro. and COMpoSitiOns: Can adVantageously be. usedin the manufacture of compositions. Comprising dispersed 0;01S fibres, 'Traditionallyõ-exploitatiOnOr the .properties of citrus fibreafoprepare a compositionAvidi excellent Theological properties requires the use of eqeipment that can imparthighto very high.
. shear during the manufactureolthe composition. Such equipment Is-usually costlyõandin operation uses a:Telativety large:amount of energy. Moreover, such higit.shear levels may be detrimental to theproperties of other constituents of such a composition. In particular if the .product is a food:product-for-instance; high shear treatment may. Adversely affect -thetaste, .
flavour and/or other organoleptieproperties provided by ober ingredients.
Osingthe -citrus.
fibres or composition in dry form comprising ohms fibres.ofthe present invention allows:Me manufactOreof intermediate or end products with dispersed Citrus fibres MAIM
requiring a.toWer amount Of -shearenergy to obtain the:saine or even better benefitsOf dispersed citrus : fibres in the manufactured product. Thus, .the citrus. fibre's. and 'composition of Matter in dry forth Of the present invention.proVide increased.flexibility and effiCieneyin stiehprodnet inamithethre;
[0001131 Consequently, the present invention in eighteenth astx..ct prOvideS a method for preparing -it composition comprising an :uqncouS Phase wherein the acitteousphase comprises dispersed citrus fibres, Wherein theinethod comprises the Step of dispersing a sou* Of citrus fibres in an aqueousinedium thereby to form at least:part of said first aqueous phase; and wherein the sour. of citrus fibres i*.citrus.fibres in dry form accoriiing to the present invention or th.ecamposition in dry krm (lewd:sing-citrus .fibrestmd an additive distributed between-said fibres according to the preseat. invention. The aqueousphase may.be prepared with a. variety of rheotogical properties, and may for instance be selected to have any consistency between-highly fluid (water thirty to a highly -viseous,. or spoonahle, or gelled consistency, Thelevel of citrus fibre in the:aqueous phase may suitably be adjusted to the Theological requirements; for the particular product Typically; the aqueous .phasemaycomprisebetween wtoiii of dispersed citrus fibreS:whh-respeet-ta the weightorthe aqueous phase, .and :prefembly-comprises between. 0,05 and ...wt-%, even More:preferably between 0.1 and 3 wt-%.of dispersed citrus fibres. ThesoitreebleithiS Mutt that isnSed in the present Method preferahly.iS acOmposition Of Matter-in:0Y rm coMprising.citrus.fibre and an additive diStributed between Said citrus fibres; It ii.partieularly preferred that: the edditiVe is:Sucrose and that the ratio A:F Of additive to citrus fibre is 0.-10-to 1.0 and 3::0 -to 1ØbY weights It is likewik preferred that the composition of citrus fibre used as the Source-Of citrus fibre -hag Fibre Availability Parameter of at least0;:79 Hz, mOrepreferably0X-Hz-and even More preferably- at least 0:9 Hz.
[0091 .141 The present method is: particularly useful in the preparation emulsified products.
Thereto* the method preferably is amethod for preparing a cem.positionin the form of an oil-= M-water.einntaion,. The oil-in-water:emulsion iS.preferablyan edible entalSion: The edible water emulsion-preferablyeoMptiseS from -5 to 59-wt.%.Of oil, The oil typically is an .edibleoit.
As understoodby the skilled person such edible oils. typically comprise triglyeeridesõusually mixtures of such fitiglycerides, Typioal esamples or edible oils includevegetable.Oils. including palm. oil, rapeseed ml linseed oil, sunflower oirand:oils-of-anintal origin.
T000115] The present method IS also. useful to prepare emulsions in the farmora dressing Ka: similar epitcligtent,..beeaut>eit to- provide rheological properties-that =generally considered destrableforõdressings, Since such dressings aretypicallyaeidiein nature, the:
.present methodi preferably forpreparingacompositionin the form. ofan Oil ;in-water emulsion :
'wherein theeompositioninthe 'bon-of:an oil-itt-water-cmalSion.comprises from.
15 to=59 wtr%
Oi land &Mt 0.1 to 1:0: Wt-%.-ofatit it is particularly preferred. that the COmpositiOn the.
form of an oil-M-Water emulsion is a Mayonnaise.
[0091 16]. The present method is also useful in the preparation ofernulsitiediproducts which comprise proteirtS/TIMS, the method is preferably a method for preparing a eompOkition in the thrill of an oil-in-water emulsion, whereinthe composition in the form .of an oil-in-Water en-Maim comprises PrOtein, wherein the amount Of protein as preferably from 0 1 to 111 wt%, more preferably from 02 to 7 wilik and even more:preferably from -0.25.to wt%
by weight of the composition; The protein :may Wyatt tage.ouslyinelude milk protein,. which is a desirable -component in manyrood eompositions. Thus ,..the protein .pteferably comprises titleast.:59 wt%
milk protein, more preferably at least 79 wt%, even more preferably at least 9q4 and still.
:morepreferablyconsists. essentially of milk protein,. The suitability of the present method. to impart desirable characteristics. deriving-from citrus fibres to an aqueous:
mediturt,,--in-the .presence of both- emulsified oil and milk protein,Anake. the method suitable for -the preparation of ready-to-drink milkteas. Hence, the present method. preferably is -method for thepreparing composition in the term of an :oit;1117!water-erntilsiOn,.Wherein:.the compositiOn inthe form of an oil- iter emulsion ita:ready4O-drinklea-based beverage.. Thetertn "ready-to-drink tea beverage" refers to a packaged lea-based beverage, i.e. a SubstanthillyaqueOus drinkable corn position stiitable for human consumption. Preferably the beVerage comprises at least 85%
water by weight of the beverageõ More preferably at let* 90%, 'Ready-kJ-drink (WM) Milk Ica .-beverages uSually-Ontain milk solids like for example milk protein and milklattitat gik;& the :beverages certain organoleptie properties like for example a tcreamy moo-111feet%. Such an RID

milk tea beverage 'preferably CoinpriSes at least 0.01 wt%-lea solids .OntMal 'weight of the.
beverage. More preferably the beverage. comprites from 004 -tO. wt% tea solids, eventriore.
preferably from 0M6 to 2% stilt more preferably from AN livt% and still even more preferably from 0.1 to 0.5'wt%. The teatolids Maybe black tensolidkgreen tea solids Ewa emnhination. theretif, The tem 4Lea Solide refers to dry material ex.traetable from the leaves and/or stemof the plant camellia .finatuis, including for example the varieties. camellia .sinensis var.; .s,klartfi,s= and/or -c:amellia shim,* var, assgmipc./. Poimples of tea solids include polypheoolsõ caffeine and amino acids. Prekrably, the are õselected .from black tea, green tea and combinations -Thereof and morepreferahlythe tea -solids are black tea soli.dsIn case. the method is .a method for thepreparation. of a ..1tTO milkteaheyerageõ--thesource-ofcitrus fibres that is used preferably is acomposition offnatterindry form -comprisingeitrus fibre and an additiye distributed between said citrus fibres. It iapartieularly preferred that theadditive sucrose:anti that the ratio A T-of.additive. to citrus fibre is 0.10 to 1.0 and -34 to. 1.0 by-weight. It:
is likewise preferred that-the composition ofeitrus ,fibre used as the source of citrus; fibrehosa Fibre Availability Parameter Of at least 070 -HZ, More preferably 0,8 Wand even more.:
-preferably alleastØ9 [000117]. The present method .is also useful fer preparing edible compositions comprisink an-aqueous phase, Which optionally -Compfise ait011-hased eonStituentõbut which. do not require 'the pre-Seri-et-Of the-Oil-based Conatintertt-'110, the present method for preparing aeotopoSitiOn wherein the composition. cornpriSes.at: least a first aqticonS phase compriSing.diapersedeitrus fibres preferably ia a method *preparing a. food emnpoSition comprising a flavoiir haSe and.
from .0 to 5. wt-iYoof oil, more preferably from 0 wt,%-to 2 .wt-%, even.
MOM preferably from .04t4igitoll WI/1;i and even more .preferablyfrom 0 10,5 wt;14 ofoil with respect to the weight .orthe composition, fierein,-Ilayour hose÷mteariathe base of the.
food composition that isrespoosible for the . identification of theproduct. The flavour haw preferably is .a.fruit-or -vegetable-based prodt.K.1,--or a.mIt.ure thereof.: The preseut-metbod is.
especially useful for imparting desirable rheological characteristics to tomatohosed products:
Therefore, more preferably: the flavour. base is a tOtnalci pAstei atemato puree, a- tomato Juice, a tomato.
concentrate or Woothinatiott thereof,: and evettntoro preferably it is:a:tomato paste. Thus, present method for preparing a composition comprising an aqueous phttSe preferablyiaa diethodforthe preparation of a composition Wherein The -Composition is it tdinato sauce or a.
--tornato. ketchup.
[000 1181 The present Method for preparing -a coMpOSitiOr4-Wherein the -Composition eotnpriseS an atlueous.phase compriSing:disperted citrus fibres 0$ *limited to the ptparation of edible Or food coMpoSitiOns.. Iheproporties of the-eitruS fibres in dry form And the composition of matter in dry form of the preSentinv.4'ntiOrt Make the present method particUlarly suitable to impart desired rheelegiral properties otith corn potitions Cottiprising asurfaCtant SyStem..Thusi: the. present -invention also provides a method the preparing a toinpOsition comprising a Surfactant System, wherein the. composition comprises at knitit alirst agnetnts phase compeising disperSed citruS fibre, wherein the method COMprises the Step of dispersing aSource of chrits.ftbres in an aqueousinediuni thereby to for* at least part of said firstaqueous phase;
and Wherein the:source-of citrus.Ores is citrus fibres in dry form according to present invention or the .composition. of matter in dry form commising citrus .fibres and additive.
distributed between stud fibres according to the presentõinvention, freferably, tht sourced citrus fibres.is a composition of matter in dry from comprising citrus:Ores and an additive distributed between. said fibres. his particularly prefeiTed that-the additive is:sucrose:and that the.
ratio A:.ofadditivetoeitrus fibre is.-0.10-mt. 1.0 and 3..0:to 1.0 by weight It is likewise preferred that the composition of eitetts fibre used as.theseurce of citrus- fibre has a FibreõAvailability Pataineter of at least 0.70-Hz.more: preferably 0.8114-andevenntore preibrablyat- least Ø9 :az.
[0001191 The tOrriposition compriaing a surfactant' systein preferably comprises the surfactant system in an artiount of OA to 504t-%, more preferably from 5I030 Wt", and. even more .prefetablyllorn 1.0 10.25 *t-% witbrespect to the weight Of the composition. There are few limitations thetype. or the. amount Of the surfactants. in general-, the surfactants may be Chosen trent the isarfactants described in .ivell-known textbooks like "Surface Active Agents L by:Schwartz & Perry, Into-Science 1949. Vol. Zhy.Se.hwartz,õPerrya, Derek Inteiseience 1958, and/or the current edition of "McCittcheon's- EtnulSitiers and Detergents"
published byManufacturing Confectioners Company orin'Tenside-Taschenbuch", H.
Stache, Ednõ Carl Hauser Vorlag,1 9$I Handbook of industrial Surfactants"14th EOn by Miehael.
Ash and Irene Ash; Synapse lrifoonationitesources, 2004. The type of spriltetant selected may depend on the type of application for which the:product is. intended. The.
surfactant system: may comprise onctype of surfactant, .or:amixtureof two or more surfactants.
Synthetic surfactants .preferably. flarra a 111410rpaS of the surfactant system. Thus, the -surfactant-system-preferably coipiise's,tieor nioresurfactants.seletted from one -ornittre of anionic surfactants, cationic.
surfactants, tonrionic surfhctants, amphoteriesurfaetantaand-zwittetionic surfactants. More preferablyOhe oric..ournore detergent surfactants, are anionie, nonionic; or a tonibinatiOnof :-artionleand nonionic Surfactants. Mixtures of synthetitanknticand noitiOnitsurfattants, Or 4 mixed siirfattant system or admix tUreaofattionic-StirfaCtkintsoionionic..-Surfaetafits.4nd atriphoterieorizwitterionic Surfactants may all benSed according to the choieeof the fOrtuulatOr for the required cleatiinit duty and the required dose of .the cleaning i.x)inpositiot.
.Preferably, the surfactant system comprisespne or more anionic Surfactartts..Maro preferably, the surfattant System comprises one or More anionic - surfactants selected from the group consisting of lauryl ether sulfates and linear alkylbenzene.sulphonates.
10001 201 For certain applications thetoMpositiOn -compriSinu'a surfactant.system:
preferably also coniprises from 1 to g Wt4,ii. of ari inorganic salt, preferably selected from.
SitlfateS-:artd. carbonate, more pmferably selected .from kig$04 and.NaiSO4 and even more-..preferably M.g-S94. The composition comprising a-SurfaCtant System maybe arty *duet comprising surfactantsõ Preferably the composition comprising a surfactant sy:stem. is -a. cleaning -compositiononore preferablya.hand dish wash composition. In view of the favourable -propertWsõthat.thepresent method õprovich* to: the composition comprising the surfactant.systemõ
the compositionpreferably further comprises. -stispendable particles andlor air hubbies.
-1000 Aecordirig*a-nineteentil aspect, the invention also relates...to:a.--conipo.sition comprisingasitraietant system wheminthecompositiOnalso -comprises the citrus fibre according .to the inventionandiorthecompositiOn ofmatter in dry form-according to the.
Invention.. -Herein; the-surfactaritsystemis as described above. The composition comprising a . surfactant systein preferably. is -aeoMposition in dry-form. Such a composition in dry form preferably eonipriSeSa.CoMpositionof Matter in dry form, wherein kildeontptiaition of matter comprises citrus fibres and an additive distributed between said.fibres. it is.partieularly preferred that the additive is siterose and. that the ratio-A :EU additive to ditrus-fibreis-0.-10 to .1 Al and -.3.0 to IAby weight.-N1ETHOP$ OF MEASUREMENT:
4.. Sample Preparation:It is. preferred that priOrto any characterization.
all-citrus -fibers' -and compositions' samples made in accordanct:with -the:Examples and Comparative Experiments presented herein below, are milledusing -Waring 801.0EG
:laboratory:
blender- (Waring Cotnmetcial, USA)-equipped With a-M.110 Pulverizer -Stainless:Steel Container using its low speedsetting -(:1-8000rinn)forIto.-5-set. Thentilled-sampleS
Were Sieved nsingn: AS200 digital shaker front Mach GrnhH Germany: with a sieve set.
of 10 mm, 500 pi, .250 pin and 50:pin:sieves (50 x -200Mmjõ.sieving etinditions 1 Min:
at amplitude Setting 60L Particles larger than 500 p'm May he milled again Until they pass.
sieve 500 pm.
Moistare:sonlent Thentoistureeontent was determined by yeighing a milled sample placed in a pre-dried vessel .ond-subseinentlytenting the vesseleornaining the 'sample overnight in an oven-at:i0.5"t;The moisture content (in wi-V)wa.s.
calculated as -(A1.-A4)/Aok100 Where Az Was the weight of the sample betbredryingirt the oven And A;1, was the weight of the resulted dried sant*, unless indicated otherwise.
. .
= Drv substance content Of. Srlistneasured :according to-formulig-.11$ (%)-----.1.0Q04... MC (%).
When the weight of anhydrous fibm in a composition needs to.bedetermined, theAbove--procedure can be Mil ized while correcting the moisture content for the additive eoritem .in-the sample.
= Standard deviation is coMputednecordingto.theibllowing formula:-Ot-is the sample mean Average and n is the sample size.
= R,* measurements:
o Sample preparation for NMR measuremeatc dispersionS-havingliber concentrations of 0,10 were prepared byrehydrating milled and sieved samples in deminerAlized water for eAchdispepion, an appropriate Amount of -sample (correcting for moistureand.additive content) was weighed. in 500 ml plastic pots and dernineralized-water was added to yield a total weightof 25Q
g, -After subsequently adding 0.24 g ofn preservative;=(Nipacide 13IT20)and -adjusting the,pH.to 34i0õ.1 using aqueous. HCE.afurther amount of dernineralized water =011$.:aati6d .4.1 yield 11,1111MUIV with a total weight of 300.g.
This mixture was homogenized at room temperature-using-a %Iverson L4RT
overhead hatch Mixer. equipped with an EntulsOr Screen (With refund: hiales:of -'abeitt I filth diameter) operated for 2 liti1-(120-se0 at 3000 rpm. The mixtures -Weke allowed to equilihrate.OVernight, after Which the pill was standardized at Using COneentrated HO.
4 Cullbrmzlwn an all4p4p(oltile testiltingpt1-$andardiz*miNture'veas transferred 'dime* to a1:/1 cm flathattain NMIttube of 10 mm diantetetat fining height of about l.cro ensuring that upon placement of the sample inthe-NMR
spectrometer, the till height is.. within the -region where the RI' .fi.ektor the coil of the NMR pertrometer ilalionogepeovs. In order to do.a background correction (calibration); Another aliquot was centrifuged (EppendocfCentrifuge 5416):tor -r01.100 a 2 tpi .Eppendort cup ata relativemuifttgatitm tbree- of 15000 to separateltte fibers from the liqUid. The top. layer (supernatant)-a the eentritliged ixture without the -fibre (hereinafterrefetted te as the "Matrix reference sample") Was. transferred-to a 18 'cut flat &Wein NMR tube at a filling height-Of 1-tin...Beth thetniktine and the MatrikretWeiitee'sainple. were incubated and equilibrated at 20 *C.: .1* 10 mm to the NMR meaSurement, The -"relative ieentrifitgal force", ri defined as r -40-/t; 'where g.=;9 ins''is the Earth's .gravitational aceeleration, r isihe rotationafradiusõpf the centrifuge, .(6 is-the angular veleeity in radians. per unit time, The angular velocity is Wr=
00, where rpm is the number nf"revolutions.per rahmte of the 0 *4M measurement; Carr Purcell N.Teibiwni Gill.(C,PM0) relaxation :decay data wereeptleeted for each mixture and :for each-matrix refer enee samPle,..A.Brulter lvlf.)20 MioiSpec: was used operating at a: resonance frequencyfor.protons of 20:
MHz; -equipped:with -a variable tern peratute. probe-head stabilized at-2.9 Measurements Were :performed Whir a CP1VIC1 T2. relaxation pulse sequence to:
Nerve the relaxation dedayat 200C (Ste -Wets f dUuwi onfive peeee..5'.idoit -Of itikkar ihitghetie Ivs'otieifirceeitporIMEria, Carr, 1-1.Y.õ Patten, PO-skid Review,. Volume 94, ISStie:3, .1954, Pages 630-638 /..Mffiedspirt-Etho .tiiehod o .theasuidng.nuckar odiattionlimesii .Melboom, S., Gilli.D,Revireivyki instraimetirs', cilpme 29; issue 8, 19584 Pageg:688-091) Data::Were Polkaed with the 1.8.1P- pulse spacing set to 200 Ps.(microseconds); a recycle .deiayThueof3Osec,a 180'-puise length of 5. PS and. using -14-.7k 1.80%pu1Ses.

The sequence deploys. g phase cycle and complex mode detection. Prior to measurement the suitability of the Nmg kyotip.fpr these measurements- (in -terms. of field homogeneity etc) was checked by verifying-that the Te of pure water was > 2ms.
a AMR data analysis az* extragtioni Data were processed with Matlab using a -singularvalue decomposition to phase correct - the quadrat:we data <"tow.ded.$
rapid and -Woe arve resolation.(06w*d-NAIR. rdaxistio v1:frail; tedinear SUCING yors us' 1)0.-:dimerisiiMill invi.fIUing .Pedersen. 141õ firo Eageben, Magr.idic Raoliairee. 081200; 157(1 Pages 141,155.
DOE 10,10060mte.2002.2570): The restating, Ohase-correded data were lertierSe-,LaplaeeTranSforated 111116.a T spectrum using the .Mattah non,=negatiVeletist isqtntrei:....enstraintqunetion 1st:111 meg (LaWS04 CL, and R.j.: Hanson, Solving -40/ .5.0a* Proplo*:Prentiee-Hallõ 1974 õ.Chapter 23, p. 161) "a boundaries .set for 12,. requiring 12 to.. be in the range of 0.01 to 10 seconds and With the regtdarizatiOn parameter lambda set to 042.
R was determined-a fallow: -titer): the T2 distribiltibti curve for 11:Pailict110r thepeakeorreSponding to the water protonglifwhich-T2 is averaged by -=exchangeberatemi the bulk Water phase and the sofa& of the fiberMaterial.
originating from the fiber MOS Was identified. Without being bound to an theory, the inventors believe that the exchange (Mid restating averaging) is due to diffusion and.themioal exchange het-won hulk and.fibersv surface sites.- The peakaot the-buik water phase are -easily distinguished, as typically they arethe peaks with the highest intensity. The peak corresponding tothe 'bulk- -water phase in the matrix reference sample was similarly-identified. The average-.1s2;
value was determined by calculating the intensity-weighted average:of:Me peak. Rsz IS
.defined as the:inverse of thisaverageTt,Le g4.-----11/32:and-is express-WOO:
The Re for a givenmixtureis altulated as the difference between -theRzoffite.
iniXtureand R-2 of the matrix rel'i.trenee sample. ThusR.* ia measurelor the bulk Water. interaction with-the .aVailabletibersurfate (ICR..BrOwnStein,-C.E.

Tarr, Journal rfMagActic Rekoilartee (1969) Volume-260.5We 1, April 1977, Pages 17-24). The characterization of the eitriislibersand compositions of the Examples atid.ComparativeEkperlinents intents:of their Re IS presented in Table te == gheajogy measurements Q Semple preparation for rheolpla meawrements.: dispersions were made by .rehydrmingin a buffer -solution the milled and -sieved samples. Dispersions with wt% and .40vit14.0hereoncentrationa were prepared. The buffer soltaon was obtained, by dissolving -40,824 grams: of 1012PO4. .2500 gut .dentineratized wow using a magnetic:Air bat The pH of the .buftbrsolutiOn-watraisoito 7.0 by.

adding drops. of SIVI NaOH solution, after which dernintralized waterWaS-addedi to obtain a total of 3000: gam Ofbtiftbr- sOlUtiOti. Each disilferSiOn was -prepared by -weighing :the-appropriate: 'amount:a:swill* (correcting for moisture- and if :applicableadditiVe-content)in500 nilplastiepots followed by addition of buffer' to a 'RAW -Weight Of 300.a. The sample was tax4-d with the -antler $41.00. tiyinittl -Stirring .ttaingaspoon....SubSequently, two different-Condition were used to facilitate the dispersion. in One Series ofexperitnents,, each aspersion was mixed widia.S.ilverson.I4RT-overhead. batch mixer equipped with an :Emulsor Screen .(with round holes 01 nun diameter) for 2 mirk at 3000 rpm. %another Seritaa eXperiments, each dispersion was treated with the same -miket-fOr I 0 Min At 8000. OM.
0 Measurements ufG'i nand kinetitatic viscosity': the -mtesuretrieitti:Veke peribernigl using an ARG2rheometer from TA iments With Sand-blasted Stainiess:steelparalled plates of 40 diameter and -operated at a temperature of 20 C using a measurement gap of 1.000 intn..To ensure:
that .measurements are carried out on. representative samples, the samples were gently stirred using a teaspoon just before placingan aliquot of the-sample in the Theometer. The Theological analysis.was%earried put using a standard protocol including atime:sweep, continuous ramps. (upand down) of the shear rate and a swain sweep -with the following ..settings;
a Time -sweep: 4elay:10s, 5min:0..1% strain at I liz;
2 :COM/NOUS ramp =stept; 0õ1:to 500 s shear rate]duration 2 min;
mode:
log sampling: -10 point/decade:
CtratinuOusramp:Ste.p2.: 5:00 WO. 1 ..s4 shear rate duration .2 Min; Mode:
logSampling: 10 pointideeade;----*. Strain sweep: Sweep: 0.1 to 500 Vcs Strain at 111-4 duration 2 Mkt; Mode:

log sampling: 10 pointidecade:
The data analysiasoftware package: form TA Instruments-allowed extracting the storage. modulus G', thekinentatie yiScosity. and theyield stress (YS). G' is reported at the-time:a :30f) seconds. The kinematic viscosity iareported ata shear -Tama 22 S (downeurve)JheYS isdeiermittedfrom the maximum in the.i graph Of G' verstis Strain%,-AndiS defined as Y-S,#. G'-:-5t strain. The charactetttatiOn ofthecitruslibers and compositions Of the Examples and COmparatEXperittionts in tents of-G% 0:SC0SW andTSõare sumMarised in Tables 2 and 3.
= Self-suspending capacity (SSC): -100infof a dispersion. wt% fibre content was prepared aspresented above hitte--"ItheOlogy:intastirenterne:.SectiOn. The dispersion =Was:carefitilypoured-to-aVoid Air entrapping, into a :100 mi.graded glass Measuring-cylinder While .keeping the cylinder slightly-tilted: Thetop of the cylinder was closed using para-film. The closed cylinder was Slowlyaliaken bYtilthigit ten tiniet-ti) 'Mix And to remove ttnY Air bubbles thattnight be trapped in Me:dispertion.
The cylinder was stored Arporif tetriperintireand.thellherS were alloWed to settle under gravity. After 24-houts,.-SSC'was...detentilnedfby measuring:the volume pecuPied-hy the fibers.-as determined by optical inspection and expressing it as a percentage from the total Volatile:
Values, are reported in Table I. The higher the volatile, the higher and thus better the --SSC-Of the saMple.
= Viscosity ratio measurements indicating the ability pfa.liber sample to develop its -funetiOnality on low shearing were made as-follows: dispersions were prepared as.
-presented ahove in the-"Rhe0ogy measurements" section.. Aft* visgogitrwas, .measured ()tithe dispersions following the methodology presented M the -¶Iilmology measurements" Subsequently, the dispersions werepas.sed through.
ahoologenizerat .250 harsõand allowed' to rest-for about I 'boor at 2t)vc to 'reach their equilibrium:state...A
second '-v isc.osity-was measured under the sameconditions aspreviouslypresented. The ratiti of thetirst viscosity 'to- the-second viseosity-is used as .8n-indicator- of the sample's capacity to reach funetiottality after1OW -shear dispersion.
[000122) The invetition-Will nOty- be described with-theitelp Ofthe following examples and comparative experiinents, Without wog however limitedThereto.

[000123) Prycimis fibers were. manalhentred as follows;-Step (1). Water was added todelieotinixod eitruspeel (aby-product ofa pectm extract ion -process)ito.ohtain an aqueons.Sl Limy having a-dry substance content of abotit.-4 wt%. The-shury-was one time charged to a pressure homogenizer (IAM" homogenizer, Ranniel 5--20,56) at 000.
-bars. An -aqueous slurry containingcitrus fibers was obtained.
Step (.2.) A .pmcipitation tank was filled with an aqueous isopropanol solution (about 82 mt% isopropanolin-water):. the aqueous slurry containing-citrus fibers was brought under . agitation into theprecipitation tank by using -a vOlumetrie pampand 0-tvecipitate in the forma granules having-sizes -between 5--mm and 50 mm was formed in the tank. The slatryikoprOpanot ratio was 1:2. AgitatiOnby.stirringwasprOVided While bringing; said starry-into the-tank and the precipitate was kept in the about 30 inimiteS:
Stop (3) The precipitate Was charged to aventriftige decanter (flonwieg terstriThge) operated at -4000 rpm, to. separate the liquid phase (i.e. Water: and iSopropatinl) from the citrus Step (4) :Steps .(2) and (3) were repeated and the precipitate as subjected to an extraction step tnincrease the dry.stthstanee .eontent. ..I.T.be_extraction step was carried outby .feeding .the precipitate-4).A screw press. The speed and pressure of the press were adjusted to: obtain a semi-dry cake havingadry substance content of about 22-.0%.

Ittp.(5) The semi-dry cake Was Comminuted using a Lodige type FM 300 DMZ
Mixer, for about 1.5 to 30-mintiteS',. to obtain mains having sizes in the -range of I in illimeter.
Step (0) The coMminuted cake was. dried in a ventilated, oven. at-40 C for about 2 hours to reach A moisture cOntent of about 8 wt%, [00012,4) The properties of the obtained .fibers are .presented in Tables l(ato.e)L.tol Figurel -Shows theTz. distribution curves roating from the inverse Laplace transform obtained daring NMR-idata analysis for the sample of Example the cogesponding matrix reference sattiple,respeetiVely,.
EXAMPLES 2 .AND-3 [0001251 Dry compositions- were manufitetured. at followst Dorn* Was::repeated with the: difference that at step:(5):-the tomtninuted semi-dry cake Was Mixed with commercial sucrose in tWO:ticreiSt:libtr rAtiOs Of 0.4:1 and -respettiVely. Betbre :adding it,The commercial .suerok Was.jjwaver* Oktitle size of ahdut 250iptit, [000/261 The properties of the obtained eompOSitionS are pi eSented hi-1'416 I (a to to 1:000.1271. Figure 2 shOwS the T,z distribution eurves reSulting front the inverse Laplace ltimsforrn obtained during NMR data atutlysis. for the StatiPle of ExainpIeZ
and the corresponding matrix reference sample, respectively:.
COMPARATIVE EXPERIMENT .1.
[0001281 A dry compositionwas manufactured.as follows:
Step (I) Water was. added to de-pectinized citrus peel to obtain an:aqueons slurry haviuga dry substance content of about :4. vvr4i-.- The slurry was charged to- 11 pressurehomogenizer (APV
hotnoueniZer, gannie 1.5.2:0,.56)..at 600 bars, An-aqueous slutry.containing eilTUS fibers was . Step (2) The aquebus Slurry containing citrus fibertWaS -subjected-to An extraction step Witha Screw press tO increase the dry Substance content to a leVel-Of about 22% wt%.
.Step (1) the setni-dry Cake waS dried on an plate in an .oV'en. at 40 C
fet:seVeral days to reach 4 Moisture content of about-8 [0001291 The properties of theobtained fibers are presented.. in Tables I
(a.V e)-toI

COMPARATIVE EXPERIMENT 2 AND 3, [000130l Dam*" of US. 6,485,767 was repeatethComitterdial Sticroselritwo.
Siteroseliber ratios and 5:1, respectively, Was LAM as additiVe and added using:a:paddle mru and ii01 for 10 'minutes: The Suerdie had an avetage partieles Size of 41164;2500) }MY.
II The properties, of the obtained -00* and compositions. are preseitted;in.Tahles 1(a.toeyto 3. Theeomparative composition hayitiga 5 1 sucrose.:flber ratio, cannot be prepared for measurements like the Other samples due to increased stickiness. and it wasdiscarded.
'SELF-SUSPENDING CAPACITY, 1.1* AND FAP VALUES
Table la SSC (%) uI
EZE
.C.E.
CE.3 Not Measurable Table lb FAP determination It2(santplei (az) itz4tuatri*) (HZ). FAP (Hz) Ex..1 0.79. 041- 0.37 0,42 0.74 [00004 .As defined in the protocol above, theTAP parameter is.detertnined on-samples prepared and analyzed in the same way as described for the method of measurement for Rt.
with the only difference being .that daringsamPlepreparation, tho,rnintares containing the Anyentivefibers-or compositions in water were hesmpgeniz.efi.at 1500:rpm.
floweyer,..it wasnot possible:to measure PAP on the samples made appordingio the comparative experiments, Awe Mese samples did not disperse well and/or did not stay-in dispersion lone :enough w allow for the;
measurement to fake:place.

[0001331 TO enable the NMR.ehataderization on the samples comparative experirnemt, R-7:* Measutehtents:Wete carried Otttoti samples dispersed at 3000:tpth rathettlian 1500 vat: The-results are presented in Table le:
.Table Ic Re* (f(.?õ) dispersing at 300 rpm 'Ex.1 1.242 Ex:õ2 1,23 0.949 CE.I 0;297 0.626 Not measurable [00013411 The factthat NMR measurements Were only:pOssible after dispersing the samples Of the comparative experiments at higher rpms (thus higher Shear) may bean indication of a larger 'available free-surface area for the fibers of the invention-then that of kniawn-ftbors, RHEOLOGY MEASUREMENTS
[pool ..SariiplOattwOnVe fihei* and compositions. Were dispersed in water by :Slitting under the.conditionsinention0 in'Tabjes 2 -and:3..-t-o obtain two fiber concentration, i.e. land -9,2 wtSõor fibers in water; respeetlyely.-Theiheology data-are presented in said Tables..Zand.
-[0001.36] k was,Oservpitat. the. inyentive-commitiQm have an optimal v iscpelastic c,g,- fewer flnetptipri ocomppsi$Gneivisepelastic..bellavior, While: the $1131W. of OK
invontiyecommaitions were-systomaticatlybelow 501.4 of-MAX,. jhoseof tho -cornparaiivc-operimags could not: even be determined since -410:omparative. sample having sucrose:act-ratio WAS not processable for the measutements, Thisis believed to-domonstrate the: abitity.of inventivatompositions to smoothen otitviscoelaaie fluctuations; which. in turn mayindicated a more teliableproeessing-therea.
[000137] It-WAS also observed that theitiVentiVe:compositions had greater Re values than -the known compdaitions-which was believed to indicate that the-addi&e is.Optimally distributed betftenthetitrtis fibers and also bet*eenthe .rnierofibrils krniina the citrus fiber.- This in turn eonfetredta the inventive composition unique *iseaelastk prOpettieS even at cOncentration.of citrus fibersas mw a ()a wtWthereby proViding-ecOnotny and ease of formulation, hiie still.
proViding the .neeeSsary. rheological behaviOr;
[MIA It was also. observed that.the inventiVetotivoSitions had greater Fibre Availability Paritmete¶FAP) values: than thektioWittomposition Which.
strengthened the belief that the additive is optimally distributed between the citrus fibers irtd ilso.:bOtween the mipmfibrilsõ forming the eittirilibersõ.
(009 in particular it wasõobserved: that it may be possible to readily disperse the in.v.entive composition by applying low Iee1s of shear (e.g. 3000 rp.10)-:and even low.C. for short.
-periods of tune 2-niinates5 While providing homogeneity and stability Oa wide yariety.of -suspensions, such 11$:11:19K-pf..1114 types used in foods, cosmetics, pharmaceaticals,. but also those used in industrial products, .Stja as. paints and muds...
[0.001401 From thepresented datacan also beobseyvetthat the fibers and compositions -made accordance with-the ye au were-410o provide optimal rhwtogical properties at extremely low toneentratiotts cg, Oa WI% In contrast thereof fibers and compositions prepared in accordance with pia art failed to. influetice:the theological 1).6W/or-a dispersions containing dietn at such low concentration.
[00041]. Moreover, although readily: dispersible at !Ow-Shear level's, the .fibers and compoMtibrisOf the invention were extremth.eflbctive in proVidingoritirimin rheolOgiCal properties to .dispersions Containing thereof also when dispersed nrideincreased shear leVelS
(e.g 0p) for longer period of time (e.g. tot*, Although herein called longer period of is he noted that 10 minutes. is Shorter-than'the time used in the prior art to disperse fibers, .[004142j .Surprisingly, all oftheaboye imentiene.d: advantages. were achieved with substantially chemically or enzyrnaticallyintinodified- citrus fibers:
'EXAMPLE 4 -ANti.COMPARATIVE EXAMPLE '4 [000.1.431 -Readylo:drink.tea beverages comprising citnislibets, homogenized with different sheattreatmenmwere prepared ash* a method according toThe invention and using a'conlparative -method, reSpecti*ely..
Citiiikfibers [000144] For Example 4. (EX.. 4), the dry eeitnpositiOtvat described in Dont* 2, comprising citrus fibers and having a sucrose content OT-28.6%.-(WW). was aged.lierbaCel -fibers were used id the comparathe example (CE4).-.
'MPata.401: 6f 0e. rea4j,..6.) .4r* mil.k.ofii [000145) Milk t.ea ingredients were. com.bined with hot Millipore water of 90 C as.defttiled in Table 4-tolbrut 800 grams ofP.,-.ady-to-drink milk tea.
Table. 4 Ingredient CE 4 EA. 4 (grains) (grams) sucrose .5136 5104 creamer 14.48 14.48 Blacks tea powder 2.15 2.1.5 Herbacel .AQ+ 0:86 Composition: of Ex-2: 1.20:
Water balance balance.
-1000141 The milk tea compositions were homogenized with anoverbead Silverson 1;40.-A: atiXer equipped with a small grid, 1 Owl boles head during .5. Minutes:A
300 nun: Part milk tea compositions was used 'to determine partieleslie direetlyaller. the Silvetgon treatment (EX. 4, and CE4, respeetiVely4and another-part:WaShotnogenized in a CivaNiro SOttvi Panda Plus High Pressure. Homogenizer in.One pass. at 250 hat .(EX. 5 and !CE5, respectively), as detailed in -Table 5.
Table 5 Shear treatment CE4 CE5 .Ex. 4 Ex. 5 SilVerS011 .11.1)11 250 bar Pairikle site matuiremOnt [000147) Pardee Sit-ea-the ready to drink' in tea saniplesTwithout any pretreattnent-such as e.g , Amieidion) was.-deterrnined With a Malvern -Mastersizef 2000 and expressed as d (01)õ.d-(0,5) and d.(09) in tatile 6.
1.099.14$1. The value Of d(0.5) isiti*diam.1*.of :the volume-equivalent sphere correspond mg to the:volume,weighted median particle volume (that is half of the total.
volume of the . material is :tp ado .up of particles. wiltfra volume: smaller than or equal to the -median volume and half of thetotal volume OfdiSperScd Material has a larger volume).
Correspondingly d(0.9).--iS the value where 90%-of the total-Volume-atilt dispersed material is made Up of particles with VelutrieS:
sinallefOr eilitatto the Volume Of a:Sphere With this diameter and d(0,1) is the valuewhere 10%
.of the total volume of the dispersed material is made up of particles withVoliinies smaller Or Oital to the volume &a Sphere with this 'diameter 'TWO.
-d (0.1.14on1 d (.15)1101 d (0.9) ) luml CE 4 30.077 79.433 17),26) Cf: 5 21531 67.250 160.153 Ex 4 0,176 23.975 87:929 EXS0.106 0.327 38,141 [0001491 The difference particle'Sie betWeed the EXamples '4 and -5 wording: to the invention andtheeoniparatie EXaMpreS CE4 and.CE5 indicates that the phYS-b*
stability of the prOdnets enmpriiing the inventiveCOmpOsition of matter in dry. font COMpriSing citrus tibreS and:
.sucrose us higher than that of the comparative .samples and that smaller particle sizes can be obtained with the inventive composition. even with the application of lower .amounts- of shear.
Thus, the examples demonstrate that the method for :preparing a composition comprising an -aqueous phase comprising dispersed citrus fibres according the invention can be used to prepare .oil-hx-water etuntsionõsuch as an RTD milk tea with favourable properties+
using a relatively limited amount of shear energy during productmanufacture.
EXAMPLES 6.AND 7 AND tOMPA.RATIVE EXAMPLES 6 and?.
[000150) Hand dishwaSh (HOW) surfactant -formulations struttuted with different citrus:
'fibre preparations were compared and investigated in: tents' Of their theological :properties.
'Exatnple 6was structured with the. thy eihns-fibresofataniple LaboVe,'Ekample.7 wii.s Structured with the coMpOSition of matter-it dry fbrirtofExaMple 2above, whieheentained -46 %sucrose.
COmparative eXturiple CE6. 'comprised non-detibrillitted: citrus "fibre (Herhiteel AQ-3-: type ..lierbaroctd, Ciertnany) Comparative Example CE7 w0,prepared withilierbacel AQ+ typeN chi*
. fibre material that was defibrillated using a high: pressure homogeniser (Panda NS1001L,fliiro7 -Soztvf, Parma, Italy) .operated at '200bar. The preparation of the samples is discussed below, :The formulations. of the .Examplecompositions.6õ: 7, CEO,' and CE7 are provided*
Table 7, 10001511 The theology of samples was analysed .with a controlled stress rhemeter (FA-AR 2000ex,TA-instruments, Delaware..PS)--fitted with a sandblasted plate geometry (sandblasted plate:diameter 40Min, gap 13.intri)-tO Obtain vist oelastie mOdall ((1') bya:time sWeep Oscillation Of 5 Min .at-20 C with a Strain of 0.1% mid frequency or I Hz.
1:0001521 in addition, the to suspend particulates swai-iilvdstigated by. stirring Iva%
.oliVe'stone abrasive .(6,30 Mesh) into aliquots .Of -etteh Of the. 4:
samples, trattSferring these in 4.
measured OlinderS, and perfOrining an accelerated Stability test :by MOM& Or the samples in a temperature regulated:cabinet-at 4'..5 (.4 At days 0õ3-õand..5.-the valarne of the Seditnented particles was:recorded-and expressed as % soctirogq; by comparison to the. total product volume; Results are presented in Table 9.
Preparation of samples:
[0061531 The hand diShwaSh-compositionit.were made following the below preparation instractions:
I Add derrii7water in abeaker.
2 Add ahetinivaient of 0-:.25A1% (darns fibre material and hydrate with overhead paddle Stirrer tbr.20- minutes (model RW27, MA-Werke, Germany).
3, Add Na01-1 While mixing.
4.- Add LAS acid while mixing.
-3: Add SLES and nix until dissOlve.d.

-6, Add preservative While mixing, k4just.014 between using:WM or chile:acid:
:8, PO-00610es .6:and 7, and comparative .example(X6: Shear the whole forth aladorrhY
srngle passage through.arripAine:Siiversonat:8000rprir using a flow-of.1100mlinibl.
9. For cOmparatie.lt Example CV: Shear the whole by single passatte through a high pressurehomogeniser at 200bar, 0, Add MgSO4.742-0.and mix until -dissolved.
Table 7 Formulations Of Ex 64 Ex7. CE64 and CE77 Ingredients Et 6 Ex 7 CE7, CES.
(%w c>c,w0 flAwt) J./mineralised water 76.98 76. 76.98 Citrus Fibre oftx. 0.25 Citrus Fibrepreparation of Ex.2 0.35 lierbaCel AQ:* tyile N 0.25 Nat)II (50%) 3.13 3.23 3.23 LAS acid (97%), 11.60 11.60 11.60 SLES 1E0 (70%) 5.36 5:36 5.36 Nipacide HIT 20 Prese0ative 0.08 0.08 0.08 Mg$0431120 1.50 2.50 2.50 Total 100.00 100.00 100.00 [000154] The resultS of the theological measurements in Table :8 show that thellOW product of CE7, structured with reference Materiel Fierhaeel AQ+ as treated above resulted in the LoWegt (7 and yield *6s Values, [0001551 The Use of pre-defibrillated citrus fibre material Of Ex. 7.in a HOW formulation and further.aetiVaticin by an in-line 'Si:Iverson mixer, significantly improved G' and yield Stress of the HPW= product.
[000.16j The highest. G' and 3,ield stress value was obtained for the Kim/
product of Ex 7, structured with the citrus filuv preparation of Ex. 2...Stabilising thepre-defibrillated primary cell wall material used in Ex 7 with sucrose clearly. further enhanced its.structuring ability upoalow:
Shear activation.
1600137] Cutuparisonshowg that Example 6 exhibited a similar Cr value as CE

7 However, Ex.:6 did not require high: pressurehomogenisation at 200 bar as CE7 did.
Table 8:13' (viscoelasfic modulus) and yield stress of UMW Droduets structured with citrus fibre Material Gt (Pa), Yield stress (Pa), a=2 CE 6 0.01 Ø03 0.023 'Ex 6 MEM 008 0,13 0.001 EMMEN ¶L" 0,24 0.004 0,06 11111 standard deviation 0001581 The accelerated suspension results of olive stones in the: HOW
products in Table 0=
show that the suspending Ability of the various samples f011owed the theological. behaviour of these saMples as Outlined in Table 8-, The higher Ibe.,0' and yield stresS
atilt sarnple,.the better its olive Stone suspending TM:vett& Ex. 7 provided the best siispension residts:

'fable 9: Accelerated suspension test at 45 C Of 'UMW .prodactt structured with citrus fibre material holding lwt% :olive Stone abrasive.Dartic16' Olive stone suspending:ability of HDW products (ml* SD) day 0 day ..3 daY5 day 15 C:E 6 3-.5* 0.7 -3.2] 4.: 0.9. -2.7 *
0.5 100 -894 0.2- :81;2 * 2.6 6.8:2 2A
Ex. I .100 --97.0-+ Q. 753 :b 01 CE 7 100 82.6.*3.2 73.1 0.2 -60.3 *- 0.9 [00Ø191. IneOttelu4Ort, it. was shown that eitras fibre material Of the present: invOritiOtt only ..regilires 1os .shear-activojon to aeliteve similar or even superior- product-strupture, -Whereas products. structured with traditional: carps. :fibre - processed in the same way, or at higher shear activation -,sbowedinferior structure.

Table 2 t..) i ¨
Rheo1ogy 1 R hi:..ology 2 ----....., ..", * .....
...
:tv, * =
* (2 minutes at 3000..rpir) .0,0 grintits at 8000 rpm) -,..:.
-.4 '../.
g; :1:9 1*
,.., .
, ____________________ P. tu 4, ...; E .e,... 0. P = at t ) u2i P-.., 11 at OW. % rl at = = ,.= .o. 0 ---, -.-- .., Q
=
;Y; = : : ro '7'''' ej ,..g. u 0 41 ba. E. til ,;-- -0. ,:¨ '''' 8 - Ci' of Of VS 21 G.' Of . of YS 22'"
t,. :0 ..---= u. .,.. ...
..c;
(Pa) U' MA (PA). 'see (Pa) G' MA (PA) .i'dc ....:
X (Pa.) X -(.Pa.) Ex.1 0:1 120 229 172 2.3 0.74 484.6 10,6 2,26 . ___________________________________ .

367(t :604.7 0 Ex.2 0.4:1 120 290 108 = 29 5,0 1.47 91 15 14.3: 2,74 0 ) 0) ..., ...

Ex.3 7:1 180 8 1279 2. 191 3.1 0.82 426,S 8.8 1.85 0 0"
i ____________________________________ , *
...
i .E..1 0:1 1440 214 0.11 604 0,004 17.95 0,2 0,10 ..."
CE,2 0.4:1 1440 314 2,59 -- 6.4 6,6/ 155.7 - .., 1.5 0.60 C8.3 5:1 4320 1256 NlY1 .N.M. -li.N. .N /NI NUM Nf.A4 _ .
(o) .,, drying time to reach the mentioned moisture content.
(*) = moisture-1i content ofthe dry composition.
9:1 en Minple's weight, 1.,e, the weight oldie dispersed dry composition in water, used for theologieal measurements. ti e (*:**)..= Citrus fibet'S.eoneOntratiOn. in the d6iters:ed composition:in water: CA
b.) (t)s' MAX
I.+
cr.
-..
o (1.1.- STDEV
4.
4.
b.) b.) Nibef "- nottueasurahie cr.

.:Tiiblo.-3.

tµ.) o _ R t16logy 1 ineoli.-,..:,y 2 --.1 4, ..-;.= ---- .i:. .-* (2 rtiltitilts: at 3000 rpm) '(.1=0-1-0.1tnitoOit 8000 rpm) --.1 '-:- 4 CA
:a ..C. ej.4 A
_______________________________________________________________________________ __ . N
f... 1; :.....,, 01 4, ) ./.-5 at,".;=.) ':',.:r,,, ' - c ...
''''' '''.73 '''". 4.t'.'''. ..4 ci .--''' .C) t T.-' YS
.11 4t \S 1:..at 2 ''',...: '';'1.' 1=;-.' 2 .--- -7. -.--,' -8 '---(i.'. of of G'. of :Of (m1 22).g.=.c :lipP .221,sec -r 45' .(P-0) G ' MA .
(PO) G' MA
:?,-A = - A r, .,-.At (Yea, 0 ' A) I. 10P.a.:.8) X.
X.
, .
.
' 'Ex.1 01 120 229 0,14 -28 4:6 2.67 208 27.1 3.903 r., E.2: 0:4:1 120 29.0 047 0,03 -/(1 50 .7.....:9 1,05 27 248 l324 .
' , ___________ ________________________________________________ , PO 7:1 180 , 8 1279 02 0,20( T ) 40 5.1. 1 .809 241 22.'3 , .3 , , t _______________________________________________________________________________ _____________________ .
.
, , .
C-E.-..-t W'1' 1440 :214 0,01 N/M .1.9 0,068:! 1.0 2.8:! , , CE.2 0.4:1 1440 314 0,07 - -1.'"ii31/4,,,i 2.3 0.0924¨ - 1,0 6,0 , _____________ C E .3 5:1 42,0 1 1256 NINI. N/M =Ni'M.
.N/M N. (M.
(6) - ctryi rqiinic to vet-1,1I the rnoistur;:: coatoro a 8%, ..C.:) -413.91.41.1r.vsattooVof.111e.::dry-voulpoitit>4.:.
Iv n -:(...*) ¨. .4p.i..00- , yll.t.,..i....illg.vgg**-0.0e-dispe.m.e.4.:4ry:oputlisp0009.= in .v.qto,. 1.1.$p:;1.for.
.t!tipcAi...3gi.01::r..41ipppr.Apt$:.
cp .=("....).--01iittgrfib6.e-totia.thiftitionliftili6 disperkit editiOcigitioiii6 =wate w o = (t)'.*:MAX
CT
-a-, .6.
.:(t)--:. T..pi...,!:v.-.6.
w w CT
:NiM*.iriot iitetable 52:

Claims